CN102974957B - Scaling powder special modified rosin and preparation method thereof - Google Patents
Scaling powder special modified rosin and preparation method thereof Download PDFInfo
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- CN102974957B CN102974957B CN201210426977.0A CN201210426977A CN102974957B CN 102974957 B CN102974957 B CN 102974957B CN 201210426977 A CN201210426977 A CN 201210426977A CN 102974957 B CN102974957 B CN 102974957B
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Abstract
The invention discloses scaling powder special modified rosin and a preparation method thereof. The scaling powder special modified rosin is made through compound, by weight, rosin 90.4%-94.8%, acrylic acid 4%-6%, fumaric acid 1%-3%, antioxidant 0.1%-0.3% and additive polonium (PO) 0.1%-0.3%. The preparation method of the scaling powder special modified rosin includes adding the rosin into a reaction still for reaction, slowly adding the fumaric acid, adding the antioxidant and the acrylic acid after the reaction is finished, sampling and detecting an acid value, cooling when the acid value is qualified, adding the additive, evenly mixing and then cooling, packaging and then obtaining the rosin. The scaling powder obtained made from the modified rosin has the advantages of not corroding base materials, so under a welding temperature, fluidity of welding flux is increased, an oxidation film on the surface of metal is eliminated, and soldering flux residues are easy to clean. Meanwhile, poisonous gas and foul smell can not be generated, and human bodies can not be damaged, and environment can not be polluted.
Description
Technical field
The present invention relates to a kind of scaling powder modified rosin and preparation method thereof.
Background technology
The welding of electronic industrial products, all adopts soldering technique mostly, and soldering technique is the quite traditional a kind of welding manner of electronic industrial products.In the welding process of soldering, colophony type scaling powder and abietyl solder are absolutely necessary, along with the quick update of electronic industrial products, the function of colophony type scaling powder also not merely requires only to have to help weldering performance, but requirement has multi-functional, scaling powder only in this way and solder could meet the fast development of electronics industry.
At present, the kind of scaling powder is a lot, can be divided into the organic and inorganic and large series of resin three substantially; Resin solder flux normally extracts from the secretion of trees, belongs to natural products, does not have what corrosivity, and rosin is the representative of this kind of solder flux, so also referred to as rosin based solder flux; Scaling powder is normally the mixture of main component with rosin, is the auxiliary material ensureing that welding process is carried out smoothly.Welding is the main processes in electronic assemblies, the auxiliary material used when scaling powder is welding, the Main Function of scaling powder is the oxide removing solder and welded mother metal surface, make the cleannes that metal surface reaches necessary, when it prevents from welding, the oxidation again on surface, reduces solder surface tension, improves welding performance, the quality of scaling powder performance, directly has influence on the quality of electronic product.
Flux ingredients mainly includes machine solvent, abietic resin and derivative thereof, synthetic resin surfactant, organic acid for activating agent, anticorrosive, cosolvent, film forming agent; Wherein, abietic resin and derivative thereof play a decisive role, and abietic resin and derivative thereof directly determine the anti-corrosive properties of scaling powder, electric insulating quality, machinery and chemical stability; Generally apply Foral as main rosin composition in the past, but in Foral application process, easily occur blushing, the quality of consequent effects electronic product.
Summary of the invention
The invention provides dedicated modified rosin of a kind of scaling powder and preparation method thereof, the dedicated modified rosin of this scaling powder is introduced in scaling powder, can solve the perishable mother metal of existing scaling powder, occur blushing, the problem of the quality of consequent effects electronic product.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
The dedicated modified rosin of scaling powder of the present invention, includes the constituent of following percentage by weight:
Rosin 90.4%-94.8%,
Acrylic acid 4%-6%,
Fumaric acid 1%-3%,
Antioxidant 0.1%-0.3%,
Auxiliary agent 0.1%-0.3%;
In technique scheme, scheme can also be more specifically: described antioxidant is alkylphenol disulfides oligomer.
Described auxiliary agent is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
The making step of the dedicated modified rosin of above-mentioned scaling powder is:
(1), the weight of rosin, acrylic acid, fumaric acid, antioxidant and auxiliary agent is weighed up respectively according to the weight percentage ranges of above-mentioned each raw material, for subsequent use;
(2) rosin, getting step (1) gained weight adds in reactor, load onto direct current condenser pipe, thermometer and agitator, pass into nitrogen, heat up, melt rosin, temperature is at 175 DEG C ~ 185 DEG C, start to stir, slowly add the fumaric acid of step (1) gained weight, then heat up, control temperature, at 200 DEG C, reacts 55 minutes ~ 65 minutes at this temperature;
(3), after step (2) reacted, add antioxidant, the acrylic acid of step (1) gained weight, continue to heat up, temperature has controlled to 235 DEG C, and back flow reaction keeps 2 hours, is now acrylic acid and fumaric acid modified rosin generation addition reaction; Continue heat up, temperature control to 250 DEG C, react 6 hours, this process is the desulphurization reaction of antioxidant, and course of reaction discharges low cut material, sampling detect acid number=220 ± 3, detect qualified after, lower the temperature, temperature controls to 220 DEG C;
(4), add the auxiliary agent of step (1) gained weight, stir, cooling discharging, obtains this modified rosin.
Rosin is a kind of acidulous material, it can remove the oxide of metal surface, and etch metal surface slightly, introducing acrylic acid is linked to the expansion that rosin contributes to solder flux, due to its extensibility and wetability good, just can reduce the solid and reliable solder joint required time of making one and temperature, this is extremely important to welding procedure.
Owing to adopting technique scheme, the present invention compared with prior art, has following beneficial effect:
1, the scaling powder obtained by this modified rosin has possessed the advantage of not corroding mother metal more, under welding temperature, can increase the mobility of solder, remove metal oxide film surface, flux residue is easily removed, and can not produce toxic gas and stink simultaneously, can not work the mischief and environmental pollution to human body.
2, owing to the addition of antioxidant and auxiliary agent, in welding, this modified rosin can have reinforcement Weldability, better reduces soldered material surface tension, auxiliary heat conduction, prevents oxidisability, improve speed of welding and clean metal, makes it surface smoothness and reaches satisfaction etc.
3, the summation of the resin acid played a major role in rosin to be a kind of molecular formula the be isomer of C19H29COOH, there is the luxuriant and rich with fragrance shelf structure of a three-membered ring, two double bonds and a carboxyl, first, under the condition of 200 DEG C of heating, rosin conjugated double bond structures and fumaric acid acid anhydride generation diels-alder reaction generate addition product, add the functionality of molecule, improve softening point, acid number, this addition product links acrylic acid again and continues addition reaction, further raising finished product acid number, interpolation antioxidant and auxiliary agent are in order to make finished product more stable, and the resin acid in this modified rosin and isodextropimaric acid are tended to balance leading position.
Detailed description of the invention
Below in conjunction with instantiation, the invention will be further described:
Embodiment 1---prepare 95.6 kilograms of dedicated modified rosin of scaling powder:
Raw material and consumption:
Rosin 90.4 kilograms,
4 kilograms, acrylic acid,
Fumaric acid 1 kilogram,
Alkylphenol disulfides oligomer 0.1 kilogram,
Four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.1 kilogram,
Preparation steps is:
(1), respectively the weight of rosin, acrylic acid, fumaric acid, alkylphenol disulfides oligomer antioxidant and four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester auxiliary agent is weighed up according to the above ratio, for subsequent use;
(2) rosin, getting 90.4 kilograms adds in reactor, load onto direct current condenser pipe, thermometer and agitator, pass into nitrogen, heat up, melt rosin, temperature is at 180 DEG C, start to stir, slowly add the fumaric acid of step 1 kilogram, then heat up, control temperature, at 200 DEG C, reacts 60 minutes at this temperature;
(3) after, step (2) has been reacted, add the alkylphenol disulfides oligomer antioxidant of 0.1 kilogram, the acrylic acid of 4 kilograms, continue to heat up, temperature controls to 235 DEG C, back flow reaction keeps 2 hours, is now acrylic acid and fumaric acid modified rosin generation addition reaction; Continue heat up, temperature control to 250 DEG C, react 6 hours, this process is the desulphurization reaction of antioxidant, and course of reaction discharges low cut material, sampling detect acid number=220 ± 3, detect qualified after, lower the temperature, temperature controls to 220 DEG C;
(4), add four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester auxiliary agent of 0.1 kilogram, stir, cooling discharging, obtains this modified rosin.
Embodiment 2---the dedicated modified rosin of preparation double centner scaling powder:
Raw material and consumption:
Rosin 92.6 kilograms,
5 kilograms, acrylic acid,
Fumaric acid 2 kilograms,
Alkylphenol disulfides oligomer 0.2 kilogram,
Four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.2 kilogram
Preparation steps is:
(1), respectively the weight of rosin, acrylic acid, fumaric acid, alkylphenol disulfides oligomer and four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester is weighed up according to the above ratio, for subsequent use;
(2) rosin, getting 92.6 kilograms adds in reactor, load onto direct current condenser pipe, thermometer and agitator, pass into nitrogen, heat up, melt rosin, temperature is at 180 DEG C, start to stir, slowly add the fumaric acid of step 2 kilogram, then heat up, control temperature, at 200 DEG C, reacts 60 minutes at this temperature;
(3) after, step (2) has been reacted, add the alkylphenol disulfides oligomer of 0.2 kilogram, the acrylic acid of 5 kilograms, continue to heat up, temperature controls to 235 DEG C, back flow reaction keeps 2 hours, is now acrylic acid and fumaric acid modified rosin generation addition reaction; Continue heat up, temperature control to 250 DEG C, react 6 hours, this process is the desulphurization reaction of antioxidant, and course of reaction discharges low cut material, sampling detect acid number=220 ± 3, detect qualified after, lower the temperature, temperature controls to 220 DEG C;
(4), add four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester of 0.2 kilogram, stir, cooling discharging, obtains this modified rosin.
Embodiment 3---prepare 104.4 kilograms of dedicated modified rosin of scaling powder:
Raw material and consumption:
Rosin 94.8 kilograms,
6 kilograms, acrylic acid,
Fumaric acid 3 kilograms,
Alkylphenol disulfides oligomer 0.3 kilogram,
Four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.3 kilogram,
Preparation steps is:
(1), respectively the weight of rosin, acrylic acid, fumaric acid, antioxidant and four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester is weighed up according to the above ratio, for subsequent use;
(2) rosin, getting 95.8 kilograms adds in reactor, load onto direct current condenser pipe, thermometer and agitator, pass into nitrogen, heat up, melt rosin, temperature is at 180 DEG C, start to stir, slowly add the fumaric acid of step 3 kilogram, then heat up, control temperature, at 200 DEG C, reacts 60 minutes at this temperature;
(3), after step (2) reacted, add the antioxidant of 0.3 kilogram, the acrylic acid of 6 kilograms, continue to heat up, temperature controls to 235 DEG C, and back flow reaction keeps 2 hours, is now acrylic acid and fumaric acid modified rosin generation addition reaction; Continue heat up, temperature control to 250 DEG C, react 6 hours, this process is the desulphurization reaction of antioxidant, and course of reaction discharges low cut material, sampling detect acid number=220 ± 3, detect qualified after, lower the temperature, temperature controls to 220 DEG C;
(4), add four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester of 0.3 kilogram, stir, cooling discharging, obtains this modified rosin.
Claims (3)
1. the dedicated modified rosin of scaling powder, is characterized in that the constituent including following percentage by weight:
Rosin 90.4%-94.8%,
Acrylic acid 4%-6%,
Fumaric acid 1%-3%,
Antioxidant 0.1%-0.3%,
Auxiliary agent 0.1%-0.3%;
Described auxiliary agent is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
2. the dedicated modified rosin of scaling powder according to claim 1, is characterized in that: described antioxidant is alkylphenol disulfides oligomer.
3. a preparation method for the dedicated modified rosin of scaling powder, is characterized in that:
Adopt the raw material of following percentage by weight:
Rosin 90.4%-94.8%,
Acrylic acid 4%-6%,
Fumaric acid 1%-3%,
Antioxidant 0.1%-0.3%,
Auxiliary agent 0.1%-0.3%;
Described auxiliary agent is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester;
Making step is:
(1), the weight of rosin, acrylic acid, fumaric acid, antioxidant and auxiliary agent is weighed up respectively according to the weight percentage ranges of above-mentioned each raw material, for subsequent use;
(2) rosin, getting step (1) gained weight adds in reactor, load onto direct current condenser pipe, thermometer and agitator, pass into nitrogen, heat up, melt rosin, temperature is at 175 DEG C ~ 185 DEG C, start to stir, slowly add the fumaric acid of step (1) gained weight, then heat up, control temperature, at 200 DEG C, reacts 55 minutes ~ 65 minutes at this temperature;
(3), after step (2) reacted, add antioxidant, the acrylic acid of step (1) gained weight, continue to heat up, temperature has controlled to 235 DEG C, and back flow reaction keeps 2 hours, is now acrylic acid and fumaric acid modified rosin generation addition reaction; Continue heat up, temperature control to 250 DEG C, react 6 hours, this process is the desulphurization reaction of antioxidant, and course of reaction discharges low cut material, sampling detect acid number=220 ± 3, detect qualified after, lower the temperature, temperature controls to 220 DEG C;
(4), add the auxiliary agent of step (1) gained weight, stir, cooling discharging, obtains this modified rosin.
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| CN201210426977.0A CN102974957B (en) | 2012-10-31 | 2012-10-31 | Scaling powder special modified rosin and preparation method thereof |
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| CN102974957B true CN102974957B (en) | 2015-04-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103212923A (en) * | 2013-05-07 | 2013-07-24 | 浙江省冶金研究院有限公司 | High temperature resistant rosinyl scaling powder |
| CN103820030B (en) * | 2014-03-05 | 2015-06-24 | 张健 | Method for preparing acrylic acid maleated rosin resin |
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| JPS6356520A (en) * | 1986-08-27 | 1988-03-11 | Showa Denko Kk | Crosslinkable compound |
| CN1579698A (en) * | 2003-08-08 | 2005-02-16 | 株式会社东芝 | Thermal-setting welding-assistant, welding paste and welding method |
| CN1872929A (en) * | 2006-05-26 | 2006-12-06 | 广西民族大学 | Method for synthesizing maleated rosin rapidly |
| CN102532495A (en) * | 2012-01-10 | 2012-07-04 | 南宁哈利玛化工有限公司 | Rosin modified composite resin and preparation method |
| CN102581523A (en) * | 2012-03-21 | 2012-07-18 | 瑞玛泰（北京）科技有限公司 | Halogen-free solder paste and preparation method thereof |
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2012
- 2012-10-31 CN CN201210426977.0A patent/CN102974957B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS6356520A (en) * | 1986-08-27 | 1988-03-11 | Showa Denko Kk | Crosslinkable compound |
| CN1579698A (en) * | 2003-08-08 | 2005-02-16 | 株式会社东芝 | Thermal-setting welding-assistant, welding paste and welding method |
| CN1313242C (en) * | 2003-08-08 | 2007-05-02 | 株式会社东芝 | Thermal-setting welding-assistant, welding paste and welding method |
| CN1872929A (en) * | 2006-05-26 | 2006-12-06 | 广西民族大学 | Method for synthesizing maleated rosin rapidly |
| CN102532495A (en) * | 2012-01-10 | 2012-07-04 | 南宁哈利玛化工有限公司 | Rosin modified composite resin and preparation method |
| CN102581523A (en) * | 2012-03-21 | 2012-07-18 | 瑞玛泰（北京）科技有限公司 | Halogen-free solder paste and preparation method thereof |
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| "富马酸改性松香树脂的合成";陈学恒;《现代化工》;20040731;第24卷;第116-119页 * |
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