CN101633721A - Polyurethane filling material for sealing electronic element - Google Patents
Polyurethane filling material for sealing electronic element Download PDFInfo
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- CN101633721A CN101633721A CN200910173019A CN200910173019A CN101633721A CN 101633721 A CN101633721 A CN 101633721A CN 200910173019 A CN200910173019 A CN 200910173019A CN 200910173019 A CN200910173019 A CN 200910173019A CN 101633721 A CN101633721 A CN 101633721A
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- propylene glycol
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Abstract
The invention discloses a polyurethane filling material for sealing an electronic element, comprising the following components: a component A and a component B, wherein the component A comprises 80-100% of polyisocyanate and 0-20% of plasticizer; the component B comprises 80-90% of end hydroxy polybutadiene, 5-10% of small molecular alcohol, 5-10% of active plasticizer and 0.01-0.1% of catalyst; and the active plasticizer is alcohol with two degrees of functionality and longer inert branch chains, and the branch chains contain ether bonds or ester groups. The component A and the component B are mixed evenly according to the mass ratio of 50:100 to 100:100. The material obtained after normal-temperature solidification has the properties that the Shao' hardness is 70-85A, the tensile strength is greater than or equal to 14MPa, the elongation rate is greater than or equal to 300%, the volume resistivity is greater than or equal to 10<15> ohm*cm, the dielectric strength is greater than or equal to 22kv/mm, and the water absorptivity is smaller than or equal to 0.14%.
Description
Technical field
The present invention relates to a kind of polyurethane filling material that is suitable for electronic component encapsulation.
Background technology
Polyurethane elastomer is good because of its insulation, water-intake rate is low, shock absorption good,, no corrosive nature bonding firmly to materials such as metals, and low, the good fluidity of viscosity before solidifying, do not contain solvent, easy to operate, be difficult for producing bubble, can operate at normal temperatures and solidify rapidly, be the ideal electronic encapsulation material.Particularly be soft section polyurethane elastomer with hydroxy-terminated polybutadienes, because its structure does not contain the ehter bond and the ester group of conventional polyurethanes, polarity is less, so have good stability to hydrolysis and excellent electrical insulation capability.In the electronic component use, it be heated the back and electronic component expand together, during cooling and electronic component shrink together, can not form the gap in insulator interface, play insulation, waterproof and dustproof, shockproof and fixed action, guarantee that electronic component and electrical equipment normally move.But present product is difficult to reach simultaneously good insulation performance, mechanical property and low water absorbable.Introduce in " preparation of self-vulcanizing two component polyurethane joint sealant " article that " plastics industry " May the 34th in 2006, the volume supplementary issue was delivered as Li Xiaojun etc., use the tensile strength of material of modified polyolefin polyvalent alcohol and modified isocyanate and reactive thinner preparation can reach 11MPa, but its volume specific resistance have only 10
11Ω cm.People such as Ding Caifeng are at " Qingtao Chemical Engineering College's journal ", introduce in the article of the 21st volume the 1st interim " development of hydroxy-terminated polybutadienes urethane electrical device pouring sealant " delivered March in 2000, use the material breakdown voltage of feedstock production such as hydroxy-terminated polybutadienes, TDI and DBP can reach 20~30kV/mm, but its tensile strength have only 5~7MPa.Introduce among the CN101058630A: pass through single stage method, the mixture of HTPB, PTMEG, BDO and the MDI of fusing are mixed, the material of preparation has mechanical property preferably after solidifying, and shortcoming is that the consistency between PTMEG, HTPB and the BDO is poor, and material is put easy layering for a long time; And added the viscosity that PTMEG can increase system, be not easy to operation; And use MDI in the prescription, and must be in advance with its fusing, can't ambient operation.Introduce among the CN101210167A: the A component that will form by 60%~80% HTPB, 10%~25% thinner, 5%~15% carbon black and mix with single stage method by 80%~95% liquefied mdi, the B component that 5%~20% catalyzer is formed, the material that obtains solidifies back draft intensity 〉=10MPa, elongation 〉=310%, volume specific resistance 〉=10
15Ω cm, dielectric strength 〉=22kV/mm.But the migration precipitation phenomenon takes place in the addition type thinner of this routine easily, causes the decline of the mechanics of materials and electric property, causes cracking phenomena occurring separating with the adhesive surface of base material, thereby loses by the protection of embedding object.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of polyurethane material that is applicable to the excellent combination property of electronic component encapsulation.This material has good insulation properties, moistureproofness, the mechanical property excellence.Can ambient cure, viscosity is low, and bubble is few, and set time is adjustable, easy handling.
Polyurethane filling material of the present invention adopts the single stage method preparation, and it is low to prepare a kind of material viscosity by the interpolation reactive plasticizer, and cured article has the polyurethane material of mechanical property preferably.This reactive plasticizer is two functionality, have the alcohols that contains ehter bond or ester group isopolarity group on longer inertia side chain and the side chain, thereby it can participate in reaction the inertia side chain is linked in the molecular structure, play internally plasticized effect, improved the elongation of material.And be difficult for separating out.The alcohol that is suitable for has: 2-pentyloxy propylene glycol, 2-octyloxy propylene glycol, the sad ester group propylene glycol of 2-etc.
Polyurethane material provided by the invention is a two-pack, in massfraction, contains following composition:
The A component is made up of 80%~100% polyisocyanates and 0%~20% softening agent.Wherein said polyisocyanates is one or both of tolylene diisocyanate, polymethylene multi-phenenyl isocyanate, preferred poly methylene poly phenyl poly isocyanate; Described softening agent is one or more in phthalate, aliphatic diacid ester class or the phosphoric acid ester, preferred phthalate, preferably o-phthalic acid dibutyl ester.
The B component is made up of the reactive plasticizer of 80%~90% hydroxy-terminated polybutadienes, 5%~10% small molecular alcohol and 5%~10% and 0.01%~0.1% catalyzer.Wherein said hydroxy-terminated polybutadienes relative molecular weight is 2000~4000; Small molecular alcohol is one or more in ethylene glycol, 1,4 butyleneglycol, 1,2 propylene glycol, the glycol ether; Reactive thinner is one or more of 2-pentyloxy propylene glycol, 2-octyloxy propylene glycol, the sad ester group propylene glycol of 2-; Catalyzer is urethane catalyzer such as stannous octoate or dibutyl tin laurate.
With A, the B component mixed by mass ratio in 50: 100~100: 100 when polyurethane material of the present invention used, and vacuumizing and defoaming is cast in around the electronic component then in case of necessity, and ambient cure gets final product.Solidifying the back material property is: hardness Shao Shi 70~85A, tensile strength 〉=14MPa, elongation 〉=300%, volume specific resistance 〉=10
15Ω cm, dielectric strength 〉=22kV/mm, and water-intake rate≤0.14%.
The preparation method of polyurethane material of the present invention is:
The preparation of A component:
With polyisocyanates at 20 ℃~30 ℃, vacuumize degassing 2~3h, discharging.As use softening agent, then at 80 ℃~100 ℃ softening agent is vacuumized dehydration in advance, be cooled to 20 ℃~30 ℃ with polyisocyanates be mixed together the degassing, discharging.
The preparation of B component
Hydroxy-terminated polybutadienes, small molecular alcohol, reactive plasticizer are added in the reactor, and 80 ℃~100 ℃ vacuumize dehydration 3~4 hours, are cooled to 60 ℃~70 ℃, add catalyzer, stir evenly, and remove steam bubble, discharging.
The electronic potting resin of background technology, its mechanical property, electric property and water-absorbent can not reach higher requirement simultaneously.The present invention under the situation that does not reduce the material electric property, has improved the mechanical property of material, and has reduced the viscosity of this system by using reactive plasticizer, and the system component consistency is good, does not have and easily separates out composition.Gained material good combination property.
Embodiment
The present invention will be further described below in conjunction with embodiment, is not limited to the present invention.
Embodiment 1:
A component: 20kg tolylene diisocyanate, 80kg polymethylene polyisocyanates at 30 ℃, are stirred evenly, remove steam bubble, discharging.
The B component: 80kg hydroxy-terminated polybutadienes (number average relative molecular weight=3000), 5kg ethylene glycol, 5kg 1,2 propylene glycol, 10kg 2-pentyloxy propylene glycol are added in the reactor, and 100 ℃ vacuumize dehydration 3h, be cooled to 60 ℃, add stannous octoate 100g, stir evenly, remove steam bubble, discharging.
Take by weighing 50kgA and 100kg B component mixing and stirring, ambient cure 7 days, it is as follows to test its performance:
Hardness: Shao Shi 85A
Tensile strength: 14.7MPa
Volume specific resistance: 2.3 * 10
15Ω cm
Dielectric strength: 22kV/mm
Water-intake rate: 0.14%
Embodiment 2:
A component: 10kg Octyl adipate, 10kg tributyl phosphate at 100 ℃, are vacuumized dehydration 2h, be cooled to 30 ℃, add 40kg tolylene diisocyanate, 40kg polymethylene polyisocyanates, stir evenly, remove steam bubble, discharging.
B component: with 85kg hydroxy-terminated polybutadienes (number average relative molecular weight=3500), 8kg ethylene glycol, 2kg 1,2 propylene glycol, 2.5kg2-octyloxy propylene glycol, the sad ester group propylene glycol of 2.5kg 2-add in the reactor, 100 ℃ vacuumize dehydration 3h, be cooled to 60 ℃, add dibutyl tin laurate 100g and stir evenly, remove steam bubble, discharging.
Take by weighing 75kgA and 100kg B component mixing and stirring, ambient cure 7 days, it is as follows to test its performance:
Hardness: Shao Shi 75A
Tensile strength: 14.0MPa
Volume specific resistance: 1.7 * 10
15Ω cm
Dielectric strength: 22kV/mm
Water-intake rate: 0.14%
Embodiment 3:
A component: the 10kg dioctyl phthalate (DOP) at 100 ℃, is vacuumized dehydration 2.5h, be cooled to 30 ℃, add the 90kg poly methylene poly phenyl poly isocyanate, stir evenly, remove steam bubble, discharging.
B component: with 80kg hydroxy-terminated polybutadienes (number average relative molecular weight=4000), 6kg ethylene glycol, 4kg 1,2 propylene glycol, 4kg 2-pentyloxy propylene glycol, 3kg2-octyloxy propylene glycol, the sad ester group propylene glycol of 3kg2-add in the reactor, 100 ℃ vacuumize dehydration 3h, be cooled to 60 ℃, add dibutyl tin laurate 10g and stir evenly, remove steam bubble, discharging.
Take by weighing 100kgA component and 100kg B component mixing and stirring, ambient cure 7 days, it is as follows to test its performance:
Hardness: Shao Shi 80A
Tensile strength: 14.1MPa
Volume specific resistance: 2.0 * 10
15Ω cm
Dielectric strength: 22V/mm
Water-intake rate: 0.1
Claims (4)
1. polyurethane filling material for sealing electronic element, contain following composition:
The A component is made up of 80%~100% polyisocyanates and 0%~20% softening agent, wherein said polyisocyanates is one or both of tolylene diisocyanate, polymethylene multi-phenenyl isocyanate, and described softening agent is one or more in phthalic ester, aliphatic diacid ester or the phosphoric acid ester;
The B component is made up of the reactive plasticizer of 80%~90% hydroxy-terminated polybutadienes, 5%~10% small molecular alcohol and 5%~10% and 0.01%~0.1% catalyzer, wherein said hydroxy-terminated polybutadienes relative molecular weight is 2000~4000, small molecular alcohol is an ethylene glycol, 1,4 butyleneglycols, 1, in 2 propylene glycol, the glycol ether one or more, reactive plasticizer is two functionality, has the alcohol that contains ehter bond or ester group on longer inertia side chain and the side chain that catalyzer is stannous octoate or dibutyl tin laurate.
2. the described polyurethane filling material of claim 1 is characterized in that reactive plasticizer is meant one or more in 2-pentyloxy propylene glycol, 2-octyloxy propylene glycol, the sad ester group propylene glycol of 2-.
3. claim 1 or 2 described polyurethane filling materials is characterized in that A, and the B component mixed by mass ratio in 50: 100~100: 100, material property is after the ambient cure: hardness Shao Shi 70~85A, tensile strength 〉=14MPa, elongation 〉=300%, volume specific resistance 〉=10
15Ω cm, dielectric strength 〉=22kV/mm, water-intake rate≤0.14%.
4. claim 1 or 2 described polyurethane filling materials is characterized in that polyisocyanates is a polymethylene multi-phenenyl isocyanate, and softening agent is a phthalic ester.
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Cited By (9)
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CN102010588A (en) * | 2010-10-25 | 2011-04-13 | 黎明化工研究院 | Low-viscosity polyurethane potting material and preparation method and use thereof |
CN102102006A (en) * | 2010-12-20 | 2011-06-22 | 东莞市宏达聚氨酯有限公司 | Method for preparing bi-component polyurethane pouring sealant and product thereof |
CN103374294A (en) * | 2012-04-25 | 2013-10-30 | 比亚迪股份有限公司 | Metalized composite, coating layer and method for selectively metallizing nonmetallic surface |
CN104448792A (en) * | 2014-12-29 | 2015-03-25 | 青岛瑞诺化工有限公司 | Electronic component encapsulating material |
CN104530366A (en) * | 2014-12-18 | 2015-04-22 | 黎明化工研究设计院有限责任公司 | Polyurethane sealing material and preparation method thereof |
CN105175674A (en) * | 2015-08-04 | 2015-12-23 | 航天材料及工艺研究所 | High hardness and high toughness polyurethane casting adhesive and application thereof |
CN107057033A (en) * | 2016-12-31 | 2017-08-18 | 广州市集友建筑材料有限公司 | A kind of polyurethane sealing material and preparation method thereof |
CN111286004A (en) * | 2020-03-31 | 2020-06-16 | 中电保力(北京)科技有限公司 | Hydrophobic polyurethane anti-condensation air-tight sealing material and preparation method thereof |
CN115322734A (en) * | 2022-09-15 | 2022-11-11 | 上海科蓝柏新材料科技有限公司 | Heat-conducting polyurethane pouring sealant, preparation method and application thereof |
Family Cites Families (4)
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GB8928157D0 (en) * | 1989-12-13 | 1990-02-14 | Bostik Ltd | Chemically-curing two-part polyurethane composition |
CN100500787C (en) * | 2006-06-26 | 2009-06-17 | 山东东大一诺威聚氨酯有限公司 | Polyurethane embedding material combination adapted for electronic component encapsulation and preparation method thereof |
CN101210167A (en) * | 2006-12-30 | 2008-07-02 | 天津市朗润思创科技发展有限公司 | Polyurethane sealing pouring adhesive and its preparing process |
CN101058630A (en) * | 2007-06-06 | 2007-10-24 | 中国科学院山西煤炭化学研究所 | Method for synthesizing urethane elastomer |
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2009
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Cited By (15)
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CN102010588A (en) * | 2010-10-25 | 2011-04-13 | 黎明化工研究院 | Low-viscosity polyurethane potting material and preparation method and use thereof |
CN102010588B (en) * | 2010-10-25 | 2012-05-23 | 黎明化工研究院 | Low-viscosity polyurethane potting material and preparation method and use thereof |
CN102102006A (en) * | 2010-12-20 | 2011-06-22 | 东莞市宏达聚氨酯有限公司 | Method for preparing bi-component polyurethane pouring sealant and product thereof |
CN102102006B (en) * | 2010-12-20 | 2013-12-11 | 东莞市宏达聚氨酯有限公司 | Method for preparing bi-component polyurethane pouring sealant and product thereof |
CN103374294A (en) * | 2012-04-25 | 2013-10-30 | 比亚迪股份有限公司 | Metalized composite, coating layer and method for selectively metallizing nonmetallic surface |
CN103374294B (en) * | 2012-04-25 | 2016-06-01 | 比亚迪股份有限公司 | One can metallized compositions, coat and the metallized method of nonmetallic surface selective |
CN104530366A (en) * | 2014-12-18 | 2015-04-22 | 黎明化工研究设计院有限责任公司 | Polyurethane sealing material and preparation method thereof |
CN104530366B (en) * | 2014-12-18 | 2017-10-13 | 黎明化工研究设计院有限责任公司 | A kind of polyurethane sealing material and preparation method thereof |
CN104448792A (en) * | 2014-12-29 | 2015-03-25 | 青岛瑞诺化工有限公司 | Electronic component encapsulating material |
CN105175674A (en) * | 2015-08-04 | 2015-12-23 | 航天材料及工艺研究所 | High hardness and high toughness polyurethane casting adhesive and application thereof |
CN107057033A (en) * | 2016-12-31 | 2017-08-18 | 广州市集友建筑材料有限公司 | A kind of polyurethane sealing material and preparation method thereof |
CN111286004A (en) * | 2020-03-31 | 2020-06-16 | 中电保力(北京)科技有限公司 | Hydrophobic polyurethane anti-condensation air-tight sealing material and preparation method thereof |
CN111286004B (en) * | 2020-03-31 | 2022-02-22 | 中电保力(北京)科技有限公司 | Hydrophobic polyurethane anti-condensation air-tight sealing material and preparation method thereof |
CN115322734A (en) * | 2022-09-15 | 2022-11-11 | 上海科蓝柏新材料科技有限公司 | Heat-conducting polyurethane pouring sealant, preparation method and application thereof |
CN115322734B (en) * | 2022-09-15 | 2024-03-29 | 上海科蓝柏新材料科技有限公司 | Heat-conducting polyurethane pouring sealant, preparation method and application thereof |
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