CN104212405A - Anti-lightning-strike polyurethane pouring sealant and preparation method - Google Patents
Anti-lightning-strike polyurethane pouring sealant and preparation method Download PDFInfo
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- CN104212405A CN104212405A CN201410358073.8A CN201410358073A CN104212405A CN 104212405 A CN104212405 A CN 104212405A CN 201410358073 A CN201410358073 A CN 201410358073A CN 104212405 A CN104212405 A CN 104212405A
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Abstract
The invention relates to a preparation method of an anti-lightning-strike polyurethane pouring sealant. The anti-lightning-strike polyurethane pouring sealant uniformly contains metal particles which accounts for 0.005-0.01% of the mass of the polyurethane pouring sealant. A material of the metal particles is iron or copper. The preparation method includes steps of: (1) preparing a polyol component from polyether polyol, epoxy resin and the metal particles; (2) carrying out a reaction to polyether polyol, epoxy resin and isocyanate with addition of a flame retardant to prepare a polyisocyanate component; and (3) mixing the polyol component with the polyisocyanate component to obtain the anti-lightning-strike polyurethane pouring sealant. The anti-lightning-strike polyurethane pouring sealant is 0.4-1.0 MPa in tensile strength, is more than 1*10<12> [omega]*M in volume resistance coefficient, allows a differential-mode 1kV voltage and a common mode 1.5kV voltage to pass, and is V0 grade in flame retardance (UL94 vertical combustion). The anti-lightning-strike polyurethane pouring sealant can be used in encapsulation of outdoor electronic elements, electronic elements in high-rise buildings and the like.
Description
Technical field
The present invention relates to polyurethane material technical field, be specifically related to a kind of anti-lightning polyurethane pouring sealant and preparation method.
Background technology
In recent years, joint sealant is widely used in the aspects such as electronic circuit, LED, electrical condenser embedding, and usage quantity rises year by year.Current Embedding Material mainly contains epoxy resin, organosilicon and urethane three major types: wherein epoxy resin joint sealant low price, adhesive property is excellent, electrical insulating property is good, but low temperature flexibility is poor, weathering resistance is poor, shrinking percentage is large; Silicone based joint sealant good flame resistance, resistant of high or low temperature are excellent, but price is high, electrical insulating property is poor; Polyurethanes joint sealant combines the advantage of epoxy resin and silicone based joint sealant, and soft durometer, curing speed regulate by formula, has excellent damping, the performance such as water-fast, wear-resisting and low temperature resistant, is widely used in embedding field.At present, the technical development of polyurethane pouring sealant is very fast, in Chinese invention patent (application number CN201010143048.X), Aerospace Material & Technology Inst. has applied for a kind of preparation method and dosing technology patent of polyurethane pouring sealant, involved joint sealant mainly good fluidity, viscosity is low, easily infiltrates to micro-aperture, is conducive to being poured thing inside and fills closely.In Chinese invention patent (application number CN201010595068.0), urethane company limited of HTC has applied for a kind of preparation method and goods patent thereof of dual-component polyurethane joint sealant, this patented product has good sticking power, snappiness, water tolerance, flame retardant resistance and electric property, is applicable to the embedding of middle-size and small-size electronic component.Other is as Beijing University of Chemical Technology Yuan Zhen " development of low in-fighting polyurethane pouring sealant " (polyurethane industrial, 2010, (1): 35-37), " development of flame-retardant polyurethane joint sealant " (Chinese sizing agent of Donghua University Li Yang, 2002,11 (2): 11-13) preparation method and the dosing technology of polyurethane pouring sealant etc. is all reported, but these conclusions be not all concerned about outdoor use particularly on Highrise buildings by the anti-lightning problem of pot electronics element, this patent is set forth just in this respect.
The electroconductibility of polyurethane material is very poor; the electric charge be trapped on polyurethane pouring sealant is broken through and the conductor gap contacted, and rushes at conductor, produces spark and even blasts; the opportunity that causing is struck by lightning causes the accident increases, and therefore causes new attention to the lightning strike protection problem of polyurethane pouring sealant.
Summary of the invention
The object of the invention is to provide a kind of anti-lightning polyurethane pouring sealant and preparation method, the polyurethane pouring sealant prepared by the method, has anti-electrostatic and assembles and diffusion spark function, and have excellent anti-lightning, water-fast, fire-retardant and low-temperature flexibility.
A kind of anti-lightning polyurethane pouring sealant comprises polyurethane pouring sealant, and evenly containing metallics in described polyurethane pouring sealant, the content of metallics is 0.005 ~ 0.01% of polyurethane pouring sealant quality.The material of described metallics is iron or copper, and particle diameter is 400 orders.
The present invention adds metallics to increase the movement of electric charge in polyurethane pouring sealant, increases anti-electrostatic and assembles and diffusion spark function; Add epoxy resin in addition, utilize the secondary hydroxyl in epoxy resin and isocyanate reaction, leave epoxide group, when meeting thunderbolt, epoxy ring-opening, sizing material gasifies, and consumes electric energy, protects the safety of electronic component internal structure.The polyurethane pouring sealant of anti-lightning performance can be applied to the embedding of outdoor, high-rise electronic component.
The concrete preparation manipulation step of anti-lightning polyurethane pouring sealant is as follows:
1) polyol component has been prepared with polyether glycol and metallics;
2) with polyether glycol, epoxy resin and isocyanate reaction, add fire retardant and prepared polyisocyanate component;
3) polyol component and polyisocyanate component are mixed to get anti-lightning polyurethane pouring sealant.
Advantageous Effects of the present invention embodies in the following areas:
(1) polyurethane pouring sealant of the present invention adopts epoxy resin, utilizes the reactivity of its secondary hydroxyl and isocyanic ester to introduce polyurethane chain, utilizes epoxide group meet thunderbolt energy-absorbing scission of link open loop and consume electric energy, to obtain anti-lightning effect;
(2) polyurethane pouring sealant of the present invention adopts metallics to assemble to obtain anti-electrostatic, thus plays the effect of anti-lightning;
(3) preparation method of polyurethane pouring sealant of the present invention, its technique is simple, and production power consumption is low, produces without " three wastes ";
(4) polyurethane pouring sealant that prepared by the present invention can be used for the embedding of the components such as outdoor electrical element, plays anti-lightning, fire-retardant, waterproof and dustproof, damping and fixing effect after solidification.
Described anti-lightning polyurethane pouring sealant salient features is in table 1:
Table 1. anti-lightning polyurethane pouring sealant salient features
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Following examples 1-4 is raw materials used to be described as follows:
Described polyether glycol is the polyether glycol containing two and above hydroxyl, as Polypropylene Oxide Triol 303 (Mn=300), Polypropylene Oxide Triol 330 (Mn=3000), polypropylene oxide glycol 220 (Mn=2000), PTMG dibasic alcohol (Mn=1000), Viscotrol C.
Described isocyanic ester is tolylene diisocyanate (TDI), isophorone diisocyanate (IPDI), hydrogenated diphenyl methane diisocyanate (H
12mDI), liquefied mdi.
Described catalyzer is metallic salt catalyzer isocyanic ester and hydroxyl reaction being had to katalysis, as dibutyl tin dilaurate.
Described fire retardant comprises reactive flame retardant and additive flame retardant, as three (chloro isopropyl) phosphoric acid ester (TCPP).
Described epoxy resin is bisphenol A type epoxy resin, and as E-44, E-51, its oxirane value is respectively 0.44,0.51.
Embodiment 1
The concrete preparation manipulation step of anti-lightning polyurethane pouring sealant is as follows:
1) polyol component is prepared:
58 grams of Polypropylene Oxide Triol 303 (Mn=300), 109 grams of Polypropylene Oxide Triol 330 (Mn=3000) and 80 grams of Viscotrol C are added, vacuum hydro-extraction 2 hours at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; Cool to less than 50 DEG C, add 1 gram of dibutyl tin dilaurate, 0.01 gram of metal iron particles, stirs, and after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
2) polyisocyanate component is prepared:
12 grams of epoxy resin E-44s are added, 75 grams of polypropylene oxide glycol 220 (Mn=2000), vacuum hydro-extraction 2 hours at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; At being cooled to 40 DEG C, add 125 grams of liquefied mdis, in 70 DEG C of reaction 4h, isocyano-content adds 81 grams of liquid flame retardants three (chloro isopropyl) phosphoric acid ester (TCPP) and stirs after reaching theoretical value, normal-temperature vacuum deaeration after 10 minutes logical nitrogen pack, obtain polyisocyanate component;
3) anti-lightning polyurethane pouring sealant is prepared:
By polyol component and polyisocyanate component in mass ratio 1:1 mix, be placed in encloses container, deaeration 15 minutes at 35 DEG C, after removing vacuum, joint sealant be poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is micro-yellow elastic body, salient features data: hardness (Shao A): 80, water-intake rate (%): 0.008, tensile strength (MPa): 0.8, elongation at break (%): 82, volume resistivity (Ω M): 1.84 × 10
13, differential mode 1kV and common mode 1.5kV voltage: pass through, flame retardant resistance (UL94 vertical combustion): V0.
Embodiment 2
74 grams of Polypropylene Oxide Triol 303 (Mn=300), 205 grams of Polypropylene Oxide Triol 330 (Mn=3000) are added, vacuum hydro-extraction 2 hours at 110 DEG C DEG C in the there-necked flask that thermometer, whipping appts are housed; Cool to less than 50 DEG C, add catalyzer 1 gram of dibutyl tin dilaurate, 0.01 gram of metallic copper particle, stirs, and after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
8 grams of epoxy resin E-44s are added, 100 grams of PTMG dibasic alcohol (Mn=1000), vacuum hydro-extraction 2 hours at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; At being cooled to 40 DEG C, add 105 grams of TDI, in 70 DEG C of reactions 4 hours, isocyano-content added 85 grams of TCPP and stirs after reaching theoretical value, normal-temperature vacuum deaeration after 10 minutes logical nitrogen pack, obtain polyisocyanate component;
By polyol component and polyisocyanate component in mass ratio 1:1 mix, be placed in encloses container, deaeration 15 minutes at 35 DEG C, after removing vacuum, joint sealant be poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is micro-yellow elastic body, salient features data: hardness (Shao A): 42, water-intake rate (%): 0.03, tensile strength (MPa): 0.45, elongation at break (%): 95, volume resistivity (Ω M): 1.66 × 10
12, differential mode 1kV and common mode 1.5kV voltage: pass through, flame retardant resistance (UL94 vertical combustion): V0.
Embodiment 3
19 grams of Polypropylene Oxide Triol 303 (Mn=300), 248 grams of Viscotrol C are added, vacuum hydro-extraction 2 hours at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; Cool to less than 50 DEG C, add catalyzer 1 gram of dibutyl tin dilaurate, 0.02 gram of metallic copper particle, stirs, and after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
13 grams of epoxy resin E-51 are added, 90 grams of polypropylene oxide glycol 220 (Mn=2000), vacuum hydro-extraction 2 hours at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; At being cooled to 40 DEG C, add 112 grams of IPDI, in 70 DEG C of reactions 5 hours, isocyano-content added 67 grams of TCPP and stirs after reaching theoretical value, normal-temperature vacuum deaeration after 10 minutes logical nitrogen pack, obtain polyisocyanate component;
By polyol component and polyisocyanate component in mass ratio 1:1 mix, be placed in encloses container, deaeration 15 minutes at 35 DEG C, after removing vacuum, joint sealant be poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is micro-yellow elastic body, salient features data: hardness (Shao A): 85, water-intake rate (%): 0.007, tensile strength (MPa): 1.0, elongation at break (%): 58, volume resistivity (Ω M): 2.1 × 10
13, differential mode 1kV and common mode 1.5kV voltage: pass through, flame retardant resistance (UL94 vertical combustion): V0.
Embodiment 4
71 grams of Polypropylene Oxide Triol 303 (Mn=300), 238 grams of Polypropylene Oxide Triol 330 (Mn=3000) are added, vacuum hydro-extraction 2 hours at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; Cool to less than 50 DEG C, add catalyzer 1 gram of dibutyl tin dilaurate, 0.02 gram of metal iron particles, stirs, and after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
13 grams of epoxy resin E-44s are added, 60 grams of PTMG dibasic alcohol (Mn=1000), vacuum hydro-extraction 2h at 110 DEG C in the there-necked flask that thermometer, whipping appts are housed; At being cooled to 40 DEG C, add 144 grams of H12MDI, in 70 DEG C of reactions 5 hours, isocyano-content added 110 grams of TCPP and stirs after reaching theoretical value, normal-temperature vacuum deaeration after 10 minutes logical nitrogen pack, obtain polyisocyanate component;
By polyol component and polyisocyanate component in mass ratio 1:1 mix, be placed in encloses container, deaeration 15 minutes at 35 DEG C, after removing vacuum, joint sealant be poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is micro-yellow elastic body, salient features data: hardness (Shao A): 60, water-intake rate (%): 0.01, tensile strength (MPa): 0.65, elongation at break (%): 87, volume resistivity (Ω M): 1.0 × 10
13, differential mode 1kV and common mode 1.5kV voltage: pass through, flame retardant resistance (UL94 vertical combustion): V0.
Claims (8)
1. an anti-lightning polyurethane pouring sealant, comprises polyurethane pouring sealant, it is characterized in that: evenly containing metallics in described polyurethane pouring sealant, the content of metallics is 0.01 ~ 0.5% of polyurethane pouring sealant quality.
2. a kind of anti-lightning polyurethane pouring sealant according to claim 1, is characterized in that: the material of described metallics is iron or copper, and particle diameter is 400 orders.
3. prepare the method for a kind of anti-lightning polyurethane pouring sealant according to claim 1, it is characterized in that concrete preparation manipulation step is as follows:
1) polyol component is prepared
By two or more polyether glycols vacuum hydro-extraction at 110 ~ 120 DEG C of 167 ~ 309 grams, cool to 50 DEG C, add the catalyzer of 1 gram, the metallics of 0.01 ~ 0.02 gram, mix, logical nitrogen is packed, and obtains polyol component;
2) polyisocyanate component is prepared:
By the polyether glycol of 60 ~ 100 grams, the epoxy resin of 8 ~ 13 grams, fire retardant vacuum hydro-extraction or drying treatment at 110 ~ 120 DEG C of 67 ~ 110 grams, cool to 40 DEG C, add the isocyanic ester of 105 ~ 144 grams, 70 ~ 80 DEG C are reacted 3 ~ 5 hours, logical nitrogen is packed, and obtains polyisocyanate component;
3) anti-lightning polyurethane pouring sealant is prepared:
By polyol component and polyisocyanate component in mass ratio 1:1 mix, be placed in encloses container, deaeration 15 minutes at 20 ~ 35 DEG C, is poured into and treats on embedding part, and room temperature is solidified or fast setting of heating for 24 hours, obtains anti-lightning polyurethane pouring sealant.
4. a kind of anti-lightning polyurethane pouring sealant according to claim 3 and preparation method, it is characterized in that: described polyether glycol is the polyether glycol containing two and above hydroxyl, as Polypropylene Oxide Triol, polypropylene oxide glycol, PTMG dibasic alcohol, Viscotrol C.
5. a kind of anti-lightning polyurethane pouring sealant according to claim 3 and preparation method, is characterized in that: described isocyanic ester is tolylene diisocyanate (TDI), isophorone diisocyanate (IPDI), hydrogenated diphenyl methane diisocyanate (H
12mDI), liquefied mdi.
6. a kind of anti-lightning polyurethane pouring sealant according to claim 3 and preparation method, is characterized in that: described catalyzer is metallic salt catalyzer isocyanic ester and hydroxyl reaction being had to katalysis, as dibutyl tin dilaurate.
7. a kind of anti-lightning polyurethane pouring sealant according to claim 3 and preparation method, is characterized in that: described fire retardant comprises reactive flame retardant and additive flame retardant, as three (chloro isopropyl) phosphoric acid ester (TCPP).
8. a kind of anti-lightning polyurethane pouring sealant according to claim 3 and preparation method, is characterized in that: described epoxy resin is bisphenol A type epoxy resin, and as E-44, E-51, its oxirane value is respectively 0.44,0.51.
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Cited By (7)
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| WO2018160217A1 (en) | 2017-03-02 | 2018-09-07 | Stepan Company | Isocyanate-modified polyester-epoxide polymer compositions |
| CN111100593A (en) * | 2019-12-31 | 2020-05-05 | 道生天合材料科技（上海）有限公司 | Epoxy resin modified high-temperature-resistant polyurethane pouring sealant |
| US10882946B2 (en) | 2016-08-25 | 2021-01-05 | Stepan Company | Polyester-epoxide polymer compositions |
| US11066550B2 (en) | 2017-03-31 | 2021-07-20 | Stepan Company | Polyether-epoxide polymer compositions |
| CN113773785A (en) * | 2021-10-19 | 2021-12-10 | 安徽匠星联创新材料科技有限公司 | Two-component polyurethane-epoxy resin pouring sealant and preparation method thereof |
| CN115595108A (en) * | 2022-10-31 | 2023-01-13 | 上海富铭密封材料有限公司（Cn） | Polyurethane pouring sealant and preparation method thereof |
| US11667821B2 (en) | 2018-12-19 | 2023-06-06 | Stepan Company | One-component adhesive compositions |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10882946B2 (en) | 2016-08-25 | 2021-01-05 | Stepan Company | Polyester-epoxide polymer compositions |
| WO2018160217A1 (en) | 2017-03-02 | 2018-09-07 | Stepan Company | Isocyanate-modified polyester-epoxide polymer compositions |
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| CN113773785A (en) * | 2021-10-19 | 2021-12-10 | 安徽匠星联创新材料科技有限公司 | Two-component polyurethane-epoxy resin pouring sealant and preparation method thereof |
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Address after: 230088 No.1, Dongmei Road, Baiyan Science Park, high tech Zone, Hefei City, Anhui Province Patentee after: Anhui Dawei Huatai New Material Technology Co.,Ltd. Address before: 230088 No.1, Dongmei Road, Baiyan Science Park, high tech Zone, Hefei City, Anhui Province Patentee before: ANHUI ANDA HUATAI NEW MATERIAL Co.,Ltd. |