CN110732804A - soldering flux for printing plate assembly and preparation method thereof - Google Patents
soldering flux for printing plate assembly and preparation method thereof Download PDFInfo
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- CN110732804A CN110732804A CN201811245700.1A CN201811245700A CN110732804A CN 110732804 A CN110732804 A CN 110732804A CN 201811245700 A CN201811245700 A CN 201811245700A CN 110732804 A CN110732804 A CN 110732804A
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- parts
- plate assembly
- printing plate
- forming agent
- film
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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
- B23K35/3612—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
- B23K35/22—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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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention provides scaling powder for printing plate assembly and a preparation method thereof, wherein the scaling powder is prepared from the following components, by weight, 24-36 parts of a film-forming agent, 2-6 parts of azoisobutyronitrile, 12-16 parts of a surfactant, 2-7 parts of stannic chloride, 3-9 parts of copper stearate, 4-8 parts of 2-amino-N-decane-acetamide, 7-11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt, 8-14 parts of dibasic lead phosphite, 6-11 parts of ammonium succinate, 7-16 parts of glutaric acid, 40-52 parts of ethylene glycol butyl ether and 36-44 parts of dimethyl adipate.
Description
Technical Field
The invention relates to the field of soldering flux, in particular to soldering flux for printing plate assembly and a preparation method thereof.
Background
With the rapid development of the electronic industry, the electronic elements, equipment and circuit design is more advanced, the process is more refined, and the requirement on the welding process of each device is higher and higher, the reliability of the welding process is crucial to ensuring the quality of the whole electronic equipment, the reliability of a welding point is the key to ensuring the product quality in the electronic industry and the instrument and meter industry, the surface tension is a main factor influencing the infiltration of the solder, which is the main function of the soldering flux is to reduce the surface tension of the solder in the welding process, film forming agents and surfactants in the soldering flux play an important role in reducing the surface tension of the solder, the wettability and the flow expansion performance of the solder can be improved, and in order to adapt to the development of the whole electronic industry and improve the welding performance, the soldering flux with good wettability, high stability and good use performance is necessary to be developed.
Disclosure of Invention
The technical problem to be solved is as follows:
the invention aims to provide soldering fluxes for printing plate assembly and a preparation method thereof, and the prepared soldering flux has high stability and no residue and can meet the requirements of industrial application.
The technical scheme is as follows:
the invention provides kinds of soldering flux for printing plate assembly, which is prepared from the following components in parts by weight:
24-36 parts of film-forming agent,
2-6 parts of azoisobutyronitrile,
12-16 parts of surfactant,
2-7 parts of tin chloride,
3-9 parts of copper stearate,
4-8 parts of 2-amino-N-decane-acetamide,
7-11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt,
8-14 parts of dibasic lead phosphite,
6-11 parts of ammonium succinate,
7-16 parts of glutaric acid,
40-52 parts of ethylene glycol butyl ether,
36-44 parts of dimethyl adipate.
Preferably, the scaling powders for printing and assembling are prepared by the following steps of dehydrating polytetrahydrofuran diol at 120 ℃ for 90min in vacuum, adding 10g of polytetrahydrofuran diol into a reactor, heating to 60 ℃, adding 18g of acetone for reacting for 20min, then dropwise adding 6g of toluene 2, 4-diisocyanate, stirring for 10min, then adding 18g of acetone, dropwise adding g of dibutyltin dilaurate, reacting for 1h while keeping the temperature, dropwise adding 1.1g of dimethylolpropionic acid, 0.4g of diethylene glycol and 3.2g of modifier, reacting for 3h, cooling to 40 ℃, adding 0.5g of triethylamine for reacting for 20min, then rapidly adding 30mL of deionized water, and decompressing and removing acetone after stirring for 1h at high speed to obtain the modified waterborne polyurethane film-forming agent.
the preferable method is that the modifier is retinol.
Preferably, the scaling powders for printing plate assembly are prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
The invention also provides a preparation method of the soldering flux for printing plate assembly, which comprises the following preparation steps:
(1) adding 40-52 parts of ethylene glycol monobutyl ether and 36-44 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, then adding 24-36 parts of a film-forming agent, 6-11 parts of ammonium succinate, 7-16 parts of glutaric acid, 2-6 parts of azoisobutyronitrile and 12-16 parts of a surfactant, and stirring for 30min under heat preservation;
(2) reducing the temperature to 50 ℃, adding 2-7 parts of stannic chloride, 3-9 parts of copper stearate, 4-8 parts of 2-amino-N-decane-acetamide, 7-11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 8-14 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing and assembling.
Has the advantages that:
(1) the invention selects the waterborne polyurethane as the film forming agent, modifies the film forming agent, and utilizes the conjugated double bond and hydroxyl structure in the retinol to improve the film forming performance of the film forming agent, so that the spreading performance of the soldering flux is better, and the thermal stability of the soldering flux is improved.
(2) The compound system of the surfactant effectively improves the wettability of the soldering flux, and the prepared soldering flux has good comprehensive performance and can meet industrial application.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The film formers of examples 1-5 and comparative example 1 were prepared by the following method:
dehydrating polytetrahydrofuran glycol at 120 ℃ for 90min in vacuum, adding 10g of polytetrahydrofuran glycol into a reactor, heating to 60 ℃, adding 18g of acetone for reacting for 20min, then dropwise adding 6g of toluene 2, 4-diisocyanate, stirring for 10min, adding 18g of acetone, dropwise adding g of dibutyltin dilaurate, reacting for 1h while keeping the temperature, dropwise adding 1.1g of dimethylolpropionic acid, 0.4g of diethylene glycol and 3.2g of retinol, reacting for 3h, cooling to 40 ℃, adding 0.5g of triethylamine for reacting for 20min, then rapidly adding 30mL of deionized water, stirring at high speed for 1h, and removing acetone under reduced pressure to obtain the modified waterborne polyurethane film-forming agent.
Example 1
(1) Adding 52 parts of ethylene glycol monobutyl ether and 36 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, adding 36 parts of a film-forming agent, 6 parts of ammonium succinate, 16 parts of glutaric acid, 2 parts of azoisobutyronitrile and 16 parts of a surfactant, and stirring for 30min at a constant temperature;
(2) and reducing the temperature to 50 ℃, adding 2 parts of tin chloride, 9 parts of copper stearate, 4 parts of 2-amino-N-decane-acetamide, 11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 8 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing plate assembly.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
Example 2
(1) Adding 40 parts of ethylene glycol monobutyl ether and 44 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, adding 24 parts of a film-forming agent, 11 parts of ammonium succinate, 7 parts of glutaric acid, 6 parts of azoisobutyronitrile and 12 parts of a surfactant, and stirring for 30min at a constant temperature;
(2) and reducing the temperature to 50 ℃, adding 7 parts of tin chloride, 3 parts of copper stearate, 8 parts of 2-amino-N-decane-acetamide, 7 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 14 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing plate assembly.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
Example 3
(1) Adding 48 parts of ethylene glycol monobutyl ether and 38 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, adding 34 parts of a film-forming agent, 7 parts of ammonium succinate, 13 parts of glutaric acid, 3 parts of azoisobutyronitrile and 15 parts of a surfactant, and stirring for 30min at a constant temperature;
(2) and reducing the temperature to 50 ℃, adding 3 parts of tin chloride, 8 parts of copper stearate, 5 parts of 2-amino-N-decane-acetamide, 10 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 10 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing plate assembly.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
Example 4
(1) Adding 44 parts of ethylene glycol monobutyl ether and 42 parts of adipic acid dimethyl ester into a reactor, uniformly mixing, heating to 65 ℃, then adding 26 parts of film-forming agent, 10 parts of succinic acid amine, 10 parts of glutaric acid, 5 parts of azoisobutyronitrile and 13 parts of surfactant, and stirring for 30min under heat preservation;
(2) and reducing the temperature to 50 ℃, adding 6 parts of tin chloride, 4 parts of copper stearate, 7 parts of 2-amino-N-decane-acetamide, 8 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 12 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing plate assembly.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
Example 5
(1) Adding 46 parts of ethylene glycol monobutyl ether and 40 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, then adding 30 parts of a film-forming agent, 8.5 parts of succinic amine, 12 parts of glutaric acid, 4 parts of azoisobutyronitrile and 14 parts of a surfactant, and stirring for 30min under heat preservation;
(2) and reducing the temperature to 50 ℃, adding 4.5 parts of tin chloride, 6 parts of copper stearate, 6 parts of 2-amino-N-decane-acetamide, 9 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 11 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing and assembling.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
Comparative example 1
The comparative example is different from example 1 in the ratio of the surfactant. Specifically, the method comprises the following steps:
(1) adding 52 parts of ethylene glycol monobutyl ether and 36 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, adding 36 parts of a film-forming agent, 6 parts of ammonium succinate, 16 parts of glutaric acid, 2 parts of azoisobutyronitrile and 16 parts of a surfactant, and stirring for 30min at a constant temperature;
(2) and reducing the temperature to 50 ℃, adding 2 parts of tin chloride, 9 parts of copper stearate, 4 parts of 2-amino-N-decane-acetamide, 11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 8 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing plate assembly.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 1:2.8: 1.9.
Comparative example 2
This comparative example differs from example 1 in that the retinol modifier is not added during the film former preparation process. Specifically, the method comprises the following steps:
(1) adding 52 parts of ethylene glycol monobutyl ether and 36 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, adding 36 parts of a film-forming agent, 6 parts of ammonium succinate, 16 parts of glutaric acid, 2 parts of azoisobutyronitrile and 16 parts of a surfactant, and stirring for 30min at a constant temperature;
(2) and reducing the temperature to 50 ℃, adding 2 parts of tin chloride, 9 parts of copper stearate, 4 parts of 2-amino-N-decane-acetamide, 11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 8 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing plate assembly.
The surfactant is prepared by mixing dibromobutenediol, cocamidopropyl betaine and dioctyl sodium sulfosuccinate according to the weight ratio of 0.7:3: 2.
The preparation method of the film forming agent comprises the steps of dehydrating polytetrahydrofuran diol at 120 ℃ for 90min in vacuum, adding 10g of polytetrahydrofuran diol into a reactor, heating to 60 ℃, adding 18g of acetone for reacting for 20min, then dropwise adding 6g of toluene 2, 4-diisocyanate, stirring for 10min, adding 18g of acetone, dropwise adding g of dibutyltin dilaurate, carrying out heat preservation reaction for 1h, cooling to 40 ℃, adding 0.5g of triethylamine for reacting for 20min, then rapidly adding 30mL of deionized water, carrying out high-speed stirring for 1h, and then carrying out reduced pressure acetone removal to obtain the modified waterborne polyurethane film forming agent.
The printing plate assembly flux prepared in examples 1 to 5 and comparative examples 1 to 2 was subjected to a performance test using an SWB-2 wetting force measuring instrument.
Appearance, physical stability test: stirring the soldering flux for a few minutes, then sealing and freezing to 6 ℃, keeping for 1 hour, observing whether layered crystals are separated out or not, judging that the surface is qualified if the phenomena do not occur, then exposing the soldering flux in a 50 ℃ oven, keeping for 1 hour, observing whether the layer is separated out or not, and judging that the surface is qualified if the layer is not separated out.
Residue dryness test: the surface is not sticky after welding, and residues on the surface are easy to remove and are regarded as qualified. The test results are given in the following table:
TABLE 1 soldering flux Performance test
According to test results, the soldering flux for printing plate assembly has a good soldering assisting effect, is stable and not layered at the low temperature of 6 ℃ and the high temperature of 50 ℃, has good spreadability, has no residue after welding, and has a high use value. The preparation method in the embodiment 5 is the optimal preparation method in the invention, the wetting time of the soldering flux prepared by the preparation method in the embodiment 5 is only 0.69s, the wetting force reaches 7.12mN, the stability is high, no residue is generated, and the industrial application requirements can be met.
Claims (5)
1, kinds of scaling powder for printing plate assembly, which is characterized by comprising the following components in parts by weight:
24-36 parts of film-forming agent,
2-6 parts of azoisobutyronitrile,
12-16 parts of surfactant,
2-7 parts of tin chloride,
3-9 parts of copper stearate,
4-8 parts of 2-amino-N-decane-acetamide,
7-11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt,
8-14 parts of dibasic lead phosphite,
6-11 parts of ammonium succinate,
7-16 parts of glutaric acid,
40-52 parts of ethylene glycol butyl ether,
36-44 parts of dimethyl adipate.
2. The flux for printing plate assembly according to claim 1, wherein the film-forming agent is prepared by the following method:
dehydrating polytetrahydrofuran glycol at 120 ℃ for 90min in vacuum, adding 10g of polytetrahydrofuran glycol into a reactor, heating to 60 ℃, adding 18g of acetone for reacting for 20min, then dropwise adding 6g of toluene 2, 4-diisocyanate, stirring for 10min, then adding 18g of acetone, dropwise adding g of dibutyltin dilaurate, reacting for 1h while keeping the temperature, dropwise adding 1.1g of dimethylolpropionic acid, 0.4g of diethylene glycol and 3.2g of modifier, reacting for 3h, cooling to 40 ℃, adding 0.5g of triethylamine for reacting for 20min, then rapidly adding 30mL of deionized water, stirring at high speed for 1h, and removing acetone under reduced pressure to obtain the modified waterborne polyurethane film-forming agent.
3. The process for preparing a film forming agent according to claim 2, wherein the modifying agent is retinol.
4. The scaling powder for printing plate assembly according to claim 1, wherein the surfactant is a mixture of dibromobutenediol, cocamidopropyl betaine, and dioctyl sodium sulfosuccinate at a weight ratio of 0.7:3: 2.
5, preparation method of the soldering flux for printing plate assembly, which is characterized by comprising the following preparation steps:
(1) adding 40-52 parts of ethylene glycol monobutyl ether and 36-44 parts of dimethyl adipate into a reactor, uniformly mixing, heating to 65 ℃, then adding 24-36 parts of a film-forming agent, 6-11 parts of ammonium succinate, 7-16 parts of glutaric acid, 2-6 parts of azoisobutyronitrile and 12-16 parts of a surfactant, and stirring for 30min under heat preservation;
(2) reducing the temperature to 50 ℃, adding 2-7 parts of stannic chloride, 3-9 parts of copper stearate, 4-8 parts of 2-amino-N-decane-acetamide, 7-11 parts of hexadecyl phenyl dimethyl quaternary ammonium salt and 8-14 parts of dibasic lead phosphite, and mixing for 40min to obtain the soldering flux for printing and assembling.
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CN201811245700.1A CN110732804A (en) | 2018-10-25 | 2018-10-25 | soldering flux for printing plate assembly and preparation method thereof |
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Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5785770A (en) * | 1996-05-30 | 1998-07-28 | Advance Research Chemicals, Inc. | Brazing flux |
CN1843684A (en) * | 2006-04-30 | 2006-10-11 | 北京市航天焊接材料厂 | Low-solid content water based clean-free welding flux without volatile organic substance and halogen |
CN101085495A (en) * | 2007-07-17 | 2007-12-12 | 西安理工大学 | Non-rosin cleaning-free scaling powder for tin-lead soldering paste and preparation method thereof |
CN101407581A (en) * | 2008-11-21 | 2009-04-15 | 东华大学 | Preparation of siloxane modified polyurethane hydrolysate |
CN101585118A (en) * | 2009-03-09 | 2009-11-25 | 郴州金箭焊料有限公司 | Soldering flux for low temperature lead-free soldering paste |
CN102199274A (en) * | 2011-04-14 | 2011-09-28 | 武汉纺织大学 | Preparation method of nanometer in situ composite reaction type organic silicone modified cationic water-based polyurethane and product thereof |
CN103881053A (en) * | 2014-04-04 | 2014-06-25 | 中南林业科技大学 | Method for preparing aqueous polyurethane emulsion modified by tung oil anhydride polyol |
CN106624464A (en) * | 2016-11-30 | 2017-05-10 | 重庆微世特电子材料有限公司 | Water-based flux |
-
2018
- 2018-10-25 CN CN201811245700.1A patent/CN110732804A/en not_active Withdrawn
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5785770A (en) * | 1996-05-30 | 1998-07-28 | Advance Research Chemicals, Inc. | Brazing flux |
CN1843684A (en) * | 2006-04-30 | 2006-10-11 | 北京市航天焊接材料厂 | Low-solid content water based clean-free welding flux without volatile organic substance and halogen |
CN101085495A (en) * | 2007-07-17 | 2007-12-12 | 西安理工大学 | Non-rosin cleaning-free scaling powder for tin-lead soldering paste and preparation method thereof |
CN101407581A (en) * | 2008-11-21 | 2009-04-15 | 东华大学 | Preparation of siloxane modified polyurethane hydrolysate |
CN101585118A (en) * | 2009-03-09 | 2009-11-25 | 郴州金箭焊料有限公司 | Soldering flux for low temperature lead-free soldering paste |
CN102199274A (en) * | 2011-04-14 | 2011-09-28 | 武汉纺织大学 | Preparation method of nanometer in situ composite reaction type organic silicone modified cationic water-based polyurethane and product thereof |
CN103881053A (en) * | 2014-04-04 | 2014-06-25 | 中南林业科技大学 | Method for preparing aqueous polyurethane emulsion modified by tung oil anhydride polyol |
CN106624464A (en) * | 2016-11-30 | 2017-05-10 | 重庆微世特电子材料有限公司 | Water-based flux |
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