CN104212405B - A kind of anti-lightning polyurethane pouring sealant and preparation method - Google Patents

A kind of anti-lightning polyurethane pouring sealant and preparation method Download PDF

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CN104212405B
CN104212405B CN201410358073.8A CN201410358073A CN104212405B CN 104212405 B CN104212405 B CN 104212405B CN 201410358073 A CN201410358073 A CN 201410358073A CN 104212405 B CN104212405 B CN 104212405B
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pouring sealant
lightning
polyurethane pouring
grams
polyurethane
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CN104212405A (en
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许戈文
熊潜生
戴震
何纪慧
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Anhui Dawei Huatai New Material Technology Co ltd
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ANHUI ANDA-HUATAI NEW MATERIAL Co Ltd
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Abstract

The preparation method that the present invention relates to a kind of anti-lightning polyurethane pouring sealant. Uniformly containing metallic in anti-lightning polyurethane pouring sealant, the content of metallic is the 0.005��0.01% of polyurethane pouring sealant quality, and the material of metallic is ferrum or copper. Preparation manipulation step is: 1) prepare polyol component with polyether polyol, epoxy resin and metallic; 2) with polyether polyol, epoxy resin and isocyanate reaction, add fire retardant and prepare polyisocyanate component; 3) polyol component and polyisocyanate component are mixed to get anti-lightning polyurethane pouring sealant. The hot strength MPa:0.4-1.0 of this anti-lightning polyurethane pouring sealant; Specific volume resistance �� M: > 1 �� 1012; Differential mode 1? kV and common mode 1.5? kV voltage: pass through; Anti-flammability UL94 vertical combustion: V0. The polyurethane pouring sealant making anti-lightning performance can apply to the embedding of the electronic component such as outdoor, skyscraper.

Description

A kind of anti-lightning polyurethane pouring sealant and preparation method
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, casting glue is widely used in the aspects such as electronic circuit, LED, capacitor embedding, and makes consumption increase year by year. Current Embedding Material mainly has epoxy resin, organosilicon and polyurethane three major types: wherein epoxy resin casting glue low price, adhesive property is excellent, electrical insulating property is good, but low temperature flexibility is poor, weatherability is poor, shrinkage factor is big; Silicone based casting glue good flame resistance, resistant of high or low temperature are excellent, but price is high, electrical insulating property is poor; Polyurethanes casting glue combines epoxy resin and the advantage of silicone based casting glue, and soft durometer, curing rate can be regulated by formula, has the damping of excellence, 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 quickly, in Chinese invention patent (application number CN201010143048.X), Aerospace Material & Technology Inst. has applied for preparation method and the dosing technology patent of a kind of polyurethane pouring sealant, involved casting glue is mainly good fluidity, viscosity is low, it is easy to penetrate into micro-aperture, is conducive to being poured the internal filling of thing closely. In Chinese invention patent (application number CN201010595068.0), polyurethane company limited of HTC has applied for preparation method and the goods patent thereof of a kind of dual-component polyurethane casting glue, this patented product has good adhesive force, pliability, resistance to water, anti-flammability and electric property, it is adaptable to the embedding of middle-size and small-size electronic component. Other is such 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 casting glue " (China's adhesive of Donghua University Li Yang, 2002,11 (2): 11-13) preparation method and the dosing technology of polyurethane pouring sealant etc. are all reported, but these conclusions use the anti-lightning problem of pot electronics element all without being concerned about on outdoor use particularly skyscraper, and this patent is illustrated by just in this respect.
The electric conductivity of polyurethane material is very poor; the electric charge being 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 the lightning strike protection problem of polyurethane pouring sealant is caused new attention.
Summary of the invention
Present invention aim at providing a kind of anti-lightning polyurethane pouring sealant and preparation method, the method polyurethane pouring sealant prepared, there is antistatic and assemble and diffusion spark function, and have the anti-lightning of excellence, water-fast, fire-retardant and low-temperature flexibility.
A kind of anti-lightning polyurethane pouring sealant includes polyurethane pouring sealant, and uniformly containing metallic in described polyurethane pouring sealant, the content of metallic is the 0.005��0.01% of polyurethane pouring sealant quality. The material of described metallic is ferrum or copper, and particle diameter is 400 orders.
The present invention adds metallic to increase the movement of electric charge in polyurethane pouring sealant, increases antistatic and assembles and diffusion spark function; It is possible to additionally incorporate epoxy resin, 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 apply to the embedding of outdoor, high-rise electronic component.
The concrete preparation manipulation step of anti-lightning polyurethane pouring sealant is as follows:
1) it is prepared for polyol component with polyether polyol and metallic;
2) with polyether polyol, epoxy resin and isocyanate reaction, add fire retardant and be prepared for polyisocyanate component;
3) polyol component and polyisocyanate component are mixed to get anti-lightning polyurethane pouring sealant.
The Advantageous Effects of the present invention is embodied in following aspect:
(1) polyurethane pouring sealant of the present invention adopts epoxy resin, utilizes the reactivity introducing polyurethane chain of its secondary hydroxyl and isocyanates, utilizes epoxide group to 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 metallic to assemble to obtain antistatic, thus playing the effect of anti-lightning;
(3) preparation method of polyurethane pouring sealant of the present invention, its technique is simple, produces power consumption low, produces without " three wastes ";
(4) polyurethane pouring sealant 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 main performance is in Table 1:
Table 1. anti-lightning polyurethane pouring sealant main performance
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
The raw materials used explanation of example 1 below-4 is as follows:
Described polyether polyol is the polyether polyol containing two and above hydroxyl, such as Polypropylene Oxide Triol 303 (Mn=300), Polypropylene Oxide Triol 330 (Mn=3000), polypropylene oxide glycol 220 (Mn=2000), PTMG dihydroxylic alcohols (Mn=1000), Oleum Ricini.
Described isocyanates is toluene di-isocyanate(TDI) (TDI), isophorone diisocyanate (IPDI), hydrogenated diphenyl methane diisocyanate (H12MDI), liquefied mdi.
Described catalyst is the metallic salt catalyst that isocyanates and hydroxyl reaction have catalytic action, such as dibutyl tin dilaurate.
Described fire retardant includes reactive flame retardant and additive flame retardant, such as three (chloro isopropyl) phosphate ester (TCPP).
Described epoxy resin is bisphenol A type epoxy resin, such as E-44, E-51, and its epoxide number 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:
Equipped with thermometer, agitating device there-necked flask in add 58 grams of Polypropylene Oxide Triol 303 (Mn=300), 109 grams of Polypropylene Oxide Triol 330 (Mn=3000) and 80 grams of Oleum Ricini, vacuum dehydration 2 hours at 110 DEG C;Cooling to less than 50 DEG C, add 1 gram of dibutyl tin dilaurate, 0.01 gram of metal iron particles, stir, after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
2) polyisocyanate component is prepared:
Equipped with thermometer, agitating device there-necked flask in add 12 grams of epoxy resin E-44s, 75 grams of polypropylene oxide glycol 220 (Mn=2000), vacuum dehydration 2 hours at 110 DEG C; It is cooled at 40 DEG C, add 125 grams of liquefied mdis, 4h is reacted in 70 DEG C, isocyano-content adds 81 grams of liquid flame retardants three (chloro isopropyl) phosphate ester (TCPP) after reaching theoretical value and stirs, after normal-temperature vacuum deaeration 10 minutes, logical nitrogen is packed, and obtains polyisocyanate component;
3) anti-lightning polyurethane pouring sealant is prepared:
Polyol component is mixed homogeneously with polyisocyanate component 1:1 in mass ratio, it is placed in hermetic container, deaeration 15 minutes at 35 DEG C, after releasing vacuum, casting glue is poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is slightly yellow elastomer, main performance data: hardness (Shao A): 80, water absorption rate (%): 0.008, hot strength (MPa): 0.8, elongation at break (%): 82, specific volume resistance (�� M): 1.84 �� 1013, differential mode 1kV and common mode 1.5kV voltage: pass through, anti-flammability (UL94 vertical combustion): V0.
Embodiment 2
Equipped with thermometer, agitating device there-necked flask in add 74 grams of Polypropylene Oxide Triol 303 (Mn=300), 205 grams of Polypropylene Oxide Triol 330 (Mn=3000), vacuum dehydration 2 hours at 110 DEG C DEG C; Cooling to less than 50 DEG C, add 1 gram of dibutyl tin dilaurate of catalyst, 0.01 gram of metallic copper particle, stir, after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
Equipped with thermometer, agitating device there-necked flask in add 8 grams of epoxy resin E-44s, 100 grams of PTMG dihydroxylic alcohols (Mn=1000), vacuum dehydration 2 hours at 110 DEG C; Being cooled at 40 DEG C, add 105 grams of TDI, react 4 hours in 70 DEG C, isocyano-content adds 85 grams of TCPP after reaching theoretical value and stirs, and after normal-temperature vacuum deaeration 10 minutes, logical nitrogen is packed, and obtains polyisocyanate component;
Polyol component is mixed homogeneously with polyisocyanate component 1:1 in mass ratio, it is placed in hermetic container, deaeration 15 minutes at 35 DEG C, after releasing vacuum, casting glue is poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is slightly yellow elastomer, main performance data: hardness (Shao A): 42, water absorption rate (%): 0.03, hot strength (MPa): 0.45, elongation at break (%): 95, specific volume resistance (�� M): 1.66 �� 1012, differential mode 1kV and common mode 1.5kV voltage: pass through, anti-flammability (UL94 vertical combustion): V0.
Embodiment 3
Equipped with thermometer, agitating device there-necked flask in add 19 grams of Polypropylene Oxide Triol 303 (Mn=300), 248 grams of Oleum Ricini, vacuum dehydration 2 hours at 110 DEG C; Cooling to less than 50 DEG C, add 1 gram of dibutyl tin dilaurate of catalyst, 0.02 gram of metallic copper particle, stir, after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
Equipped with thermometer, agitating device there-necked flask in add 13 grams of epoxy resin E-51,90 grams of polypropylene oxide glycol 220 (Mn=2000), vacuum dehydration 2 hours at 110 DEG C;Being cooled at 40 DEG C, add 112 grams of IPDI, react 5 hours in 70 DEG C, isocyano-content adds 67 grams of TCPP after reaching theoretical value and stirs, and after normal-temperature vacuum deaeration 10 minutes, logical nitrogen is packed, and obtains polyisocyanate component;
Polyol component is mixed homogeneously with polyisocyanate component 1:1 in mass ratio, it is placed in hermetic container, deaeration 15 minutes at 35 DEG C, after releasing vacuum, casting glue is poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is slightly yellow elastomer, main performance data: hardness (Shao A): 85, water absorption rate (%): 0.007, hot strength (MPa): 1.0, elongation at break (%): 58, specific volume resistance (�� M): 2.1 �� 1013, differential mode 1kV and common mode 1.5kV voltage: pass through, anti-flammability (UL94 vertical combustion): V0.
Embodiment 4
Equipped with thermometer, agitating device there-necked flask in add 71 grams of Polypropylene Oxide Triol 303 (Mn=300), 238 grams of Polypropylene Oxide Triol 330 (Mn=3000), vacuum dehydration 2 hours at 110 DEG C; Cooling to less than 50 DEG C, add 1 gram of dibutyl tin dilaurate of catalyst, 0.02 gram of metal iron particles, stir, after normal-temperature vacuum deaeration, logical nitrogen is packed, and obtains polyol component;
Equipped with thermometer, agitating device there-necked flask in add 13 grams of epoxy resin E-44s, 60 grams of PTMG dihydroxylic alcohols (Mn=1000), vacuum dehydration 2h at 110 DEG C; Being cooled at 40 DEG C, add 144 grams of H12MDI, react 5 hours in 70 DEG C, isocyano-content adds 110 grams of TCPP after reaching theoretical value and stirs, and after normal-temperature vacuum deaeration 10 minutes, logical nitrogen is packed, and obtains polyisocyanate component;
Polyol component is mixed homogeneously with polyisocyanate component 1:1 in mass ratio, it is placed in hermetic container, deaeration 15 minutes at 35 DEG C, after releasing vacuum, casting glue is poured in mould, at 50 DEG C 20 minutes namely curable, obtain anti-lightning polyurethane pouring sealant.
Anti-lightning polyurethane pouring sealant is slightly yellow elastomer, main performance data: hardness (Shao A): 60, water absorption rate (%): 0.01, hot strength (MPa): 0.65, elongation at break (%): 87, specific volume resistance (�� M): 1.0 �� 1013, differential mode 1kV and common mode 1.5kV voltage: pass through, anti-flammability (UL94 vertical combustion): V0.

Claims (6)

1. an anti-lightning polyurethane pouring sealant, including polyurethane pouring sealant, it is characterised in that: uniformly containing metallic in described polyurethane pouring sealant, the material of described metallic is ferrum or copper, and particle diameter is 400 orders;
The concrete operation step preparing a kind of anti-lightning polyurethane pouring sealant is as follows:
1) polyol component is prepared
By two or more polyether polyol vacuum dehydration at 110��120 DEG C of 167��309 grams, cooling to 50 DEG C, add the catalyst of 1 gram, the metallic of 0.01��0.02 gram, mix homogeneously, logical nitrogen is packed, and obtains polyol component;
2) polyisocyanate component is prepared:
By the polyether polyol of 60��100 grams, the epoxy resin of 8��13 grams, fire retardant vacuum dehydration at 110��120 DEG C of 67��110 grams, cooling to 40 DEG C, add the isocyanates 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 1:1 mix homogeneously in mass ratio, it is placed in hermetic container, deaeration 15 minutes at 20��35 DEG C, it is poured into and treats on embedding part, room temperature solidifies or heats fast setting for 24 hours, obtains anti-lightning polyurethane pouring sealant.
2. a kind of anti-lightning polyurethane pouring sealant according to claim 1, it is characterized in that: described polyether polyol is the polyether polyol containing two and above hydroxyl, be specially Polypropylene Oxide Triol, polypropylene oxide glycol, PTMG dihydroxylic alcohols, Oleum Ricini.
3. a kind of anti-lightning polyurethane pouring sealant according to claim 1, it is characterised in that: described isocyanates is toluene di-isocyanate(TDI) (TDI), isophorone diisocyanate (IPDI), hydrogenated diphenyl methane diisocyanate (H12MDI), liquefied mdi.
4. a kind of anti-lightning polyurethane pouring sealant according to claim 1, it is characterised in that: described catalyst is the metallic salt catalyst that isocyanates and hydroxyl reaction have catalytic action, is specially dibutyl tin dilaurate.
5. a kind of anti-lightning polyurethane pouring sealant according to claim 1, it is characterised in that: described fire retardant includes reactive flame retardant and additive flame retardant, is specially three (chloro isopropyl) phosphate ester (TCPP).
6. a kind of anti-lightning polyurethane pouring sealant according to claim 1, it is characterised in that: described epoxy resin is bisphenol A type epoxy resin, is specially E-44, E-51, its epoxide number respectively 0.44,0.51.
CN201410358073.8A 2013-12-16 2014-07-25 A kind of anti-lightning polyurethane pouring sealant and preparation method Active CN104212405B (en)

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CN109661417B (en) 2016-08-25 2021-07-16 斯泰潘公司 Polyester-epoxy polymer composition
WO2018160217A1 (en) 2017-03-02 2018-09-07 Stepan Company Isocyanate-modified polyester-epoxide polymer compositions
WO2018182770A1 (en) 2017-03-31 2018-10-04 Stepan Company Polyether-epoxide polymer compositions
EP3898758A1 (en) 2018-12-19 2021-10-27 Stepan Company One-component adhesive compositions
CN111100593B (en) * 2019-12-31 2022-01-07 道生天合材料科技(上海)股份有限公司 Epoxy resin modified high-temperature-resistant polyurethane pouring sealant
CN113773785B (en) * 2021-10-19 2023-06-16 安徽匠星联创新材料科技有限公司 Double-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

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WO2012084937A1 (en) * 2010-12-24 2012-06-28 Sika Technology Ag Adhesive for rotor blades for wind power plants
CN103013421A (en) * 2012-12-06 2013-04-03 常熟国和新材料有限公司 Solvent-free polyurethane compound adhesive and preparation method thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
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WO2012084937A1 (en) * 2010-12-24 2012-06-28 Sika Technology Ag Adhesive for rotor blades for wind power plants
CN103013421A (en) * 2012-12-06 2013-04-03 常熟国和新材料有限公司 Solvent-free polyurethane compound adhesive and preparation method thereof

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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.