CN101928377B - Flame retardant polyurethane pouring sealant, preparation method thereof and using method thereof - Google Patents
Flame retardant polyurethane pouring sealant, preparation method thereof and using method thereof Download PDFInfo
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- CN101928377B CN101928377B CN 201010278348 CN201010278348A CN101928377B CN 101928377 B CN101928377 B CN 101928377B CN 201010278348 CN201010278348 CN 201010278348 CN 201010278348 A CN201010278348 A CN 201010278348A CN 101928377 B CN101928377 B CN 101928377B
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Abstract
The invention relates to flame retardant polyurethane pouring sealant, a preparation method thereof and a using method thereof. The flame retardant polyurethane pouring sealant consists of a component A and a component B in a weight ratio of 100:60-65. The component A consists of the following raw materials in part by weight: 60 to 75 parts of oligomer polyol, 0.1 part of catalyst, 0.4 part of stabilizer, 0.5 part of defoaming agent and 24 to 39 parts of liquid flame retardant. The component B is isocyanate. The flame retardant polyurethane pouring sealant does not contain plasticizer and therefore is very environmentally-friendly and flame retardant; and the flame retardant polyurethane pouring sealant is cheap and less viscous. The double-component system can be cured at room temperature or by heating, so the operation is simple. The preparation process technique is simple. The cured polyurethane pouring sealant material has environmentally-friendly, flame-retarding, elastic, transparent and low-hardness performance as well as high bonding force with various material, good electrical property and low temperature flexibility.
Description
Technical field
The present invention relates to a kind of joint sealant and preparation method thereof and method of use, relate in particular to a kind of flame retardant polyurethane pouring sealant and preparation method thereof and method of use.
Background technology
The application of joint sealant more and more widely can be divided into epoxy pouring sealant, organic silicon potting adhesive, polyurethane pouring sealant etc. by system, is divided into transparent, heat conduction, joint sealant such as fire-retardant by application, and various joint sealants respectively have superiority, and shortcoming is respectively arranged.Epoxy systems force of cohesion is excessive; The organic silicon potting adhesive price is high, and intensity is low, and is water-fast poor.And urethane can have higher elasticity and intensity in the durometer level of broad, its excellent abrasive, oil-proofness, resistance to fatigue, anti-vibration resistance, water tolerance, excellent electrical insulation capability; Cheap price makes its wiring board at various units, high voltage capacitor; RF, high tension coil, high efficiency filter; Outdoor display screen, outdoor lamp is used widely on the wiring boards such as power module such as HID; Polyurethane pouring sealant plays sealing and protection to various components and parts, avoids the effect of the influence of moisture, machinery and environment.
Most of polyurethane pouring sealant because problems such as viscosity, proportioning, cost all contain softening agent, does not meet the environmental protection standard of European Union, and polyurethane material can discharge toxic gas when burning.
Summary of the invention
The present invention is directed to most of polyurethane pouring sealant; Because problems such as viscosity, proportioning, cost all contain softening agent, do not meet the environmental protection standard of European Union; And polyurethane material is when burning; Can discharge the deficiency of toxic gas, a kind of flame retardant polyurethane pouring sealant that is applicable to electronics and electrical component and preparation method thereof and method of use are provided, the polyurethane pouring sealant that makes not plasticizer-containing, have fire-retardant, two components, LV, transparent, environmental protection, sticking power excellence and the low advantage of cost.
The technical scheme that the present invention solves the problems of the technologies described above is following: a kind of flame retardant polyurethane pouring sealant is that the first component and the second component of 100:60～65 formed by weight proportion; Said first component is made up of the raw material of following parts by weight: 60 parts～75 parts oligomer polyol, 0.1 part catalyzer, 0.4 part stablizer, 0.5 part skimmer, 24 parts～39 parts liquid flame retardant; Said second component is an isocyanic ester.
The invention has the beneficial effects as follows: the fire retardant that adopts natural Viscotrol C and response type is a reactant, does not add softening agent, very environmental protection, fire-retardant, and also price is low, and viscosity is low.Adopt both ambient temperature curables of bicomponent system, can be heating and curing again, easy and simple to handle.The preparation process is simple.Polyurethane potting material after the curing has environmental protection, fire-retardant, elasticity, transparent, soft concurrently, various materials is had good bonding force, the performance of good electrical properties and low temperature flexibility.
On the basis of technique scheme, the present invention can also do following improvement.
Further, said oligomer polyol is hydroxy-terminated polybutadienes or Viscotrol C, and preferably, said oligomer polyol is cheap Viscotrol C.
Further, said catalyzer comprises a kind of or any several kinds mixture in dibutyl tin laurate, stannous octoate, three Bismuth Octoates and three bismuth valerates, and preferably, said catalyzer is a stannous octoate.
Further, said stablizer is antioxidant 1010 and UV light absorber UV-327.
The chemistry of said antioxidant 1010 is called four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester.The staple of said UV light absorber UV-327 is 2-(2'-hydroxyl-3', 5'-di-tert-butyl-phenyl)-5-chlorinated benzotriazole, and it is the remarkable efficient anti-aging auxiliary agent of performance; Can absorb the ultraviolet ray of 300-400 millimeter consumingly, the highest absorption peak is 353 millimicrons, and chemicalstability is good; Volatility is little; Good with polyolefinic intermiscibility, be specially adapted to Vilaterm and Vestolen PP 7052, also can be used for polyoxymethylene, gather methyl and olefin(e) acid methyl esters, many fields such as urethane, polypropylene fiber.
Further, said skimmer comprises a kind of or any several kinds mixture in non-silicone high molecular polymer, modified polyorganosiloxane and the acrylic ester copolymerization thing, and preferably, said skimmer is a modified polyorganosiloxane, as moral modest 5500.
Further; Said liquid flame retardant comprises reactive-type flame retardant and nonactive fire retardant; Preferably, said liquid flame retardant is active phosphonium flame retardant, joins phosphorous, nitrogen reactive-type flame retardant FR-lm6 (phosphorous 12.4%), the FR-600 (phosphorous 13.7%) beautify the worker like Qingdao.。
Further, said isocyanic ester comprises 2,4-diphenylmethanediisocyanate and 4,4-mixtures of diisocyanates and diphenylmethane (MDI-50), poly methylene poly phenyl poly isocyanate.A kind of or any several kinds mixture in liquefied mdi and the isoflurane chalcone diisocyanate preferably, is selected reacting balance, low viscous 2 for use, 4-diphenylmethanediisocyanate and 4,4-mixtures of diisocyanates and diphenylmethane (MDI-50).
The present invention also provides a kind of technical scheme that solves the problems of the technologies described above following: a kind of preparation method of flame retardant polyurethane pouring sealant comprises: at first, make first component and second component; Then; Is that 100:60～65 mix and get final product with first component and second component according to weight proportion; The preparation of said first component comprises oligomer polyol, catalyzer, stablizer, skimmer and liquid flame retardant is joined in the reaction kettle; Heat while stirring, when being heated to 110 ℃～120 ℃ under vacuum condition dry 2 hours, again under protection of nitrogen gas after the cooling; Pack and get final product, the preparation of said second component comprises isocyanic ester mixed directly to pack under protection of nitrogen gas and gets final product.
The present invention also provides a kind of technical scheme that solves the problems of the technologies described above following: a kind of method of use of flame retardant polyurethane pouring sealant comprises: at first, will treat that the embedding part carries out drying treatment; Then, above-mentioned flame retardant polyurethane pouring sealant is poured into treats on the embedding part, at room temperature solidifying 24 hours or being heating and curing and gets final product.When using flame retardant polyurethane pouring sealant of the present invention, first component and second component are mixed, if necessary, carry out vacuum defoamation after mixing again.
Embodiment
Below principle of the present invention and characteristic are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Embodiment 1
First component: Viscotrol C 72 weight parts, fire retardant FR-lm6 27 weight parts, inferior tin 0.1 weight part of octoate catalyst, antioxidant 1010 0.2 weight part, UV light absorber UV-327 0.2 weight part are added in the still; Be heated to 110 ℃～120 ℃; Vacuum-drying 2 hours; Nitrogen protection adds skimmer 5,500 0.5 weight parts down, mixes the nitrogen protection bottom discharge.
Second component: MDI-50 is with respect to first component 60 weight parts.
First and second components are mixed back (vacuum defoamation in case of necessity) with the weight ratio of 100:60 make sample to be tested.
Embodiment 2
First component: Viscotrol C 62 weight parts, fire retardant FR-lm6 37 weight parts, catalyzer dibutyl tin laurate 0.1 weight part, antioxidant 1010 0.2 weight part, UV light absorber UV-327 0.2 weight part are added in the still; Be heated to the 110-120 degree; Vacuum-drying 2 hours; Nitrogen protection adds skimmer 5,500 0.5 weight parts down, mixes the nitrogen protection bottom discharge.
Second component: MDI-50 is with respect to first component 65 weight parts.
First and second components are mixed back (vacuum defoamation in case of necessity) with the weight ratio of 100:65 make sample to be tested.
Embodiment 3
First component: Viscotrol C 60 weight parts, fire retardant FR-600 37 weight part, inferior tin 0.1 weight part of octoate catalyst, antioxidant 1010 0.2 weight part, UV light absorber UV-327 0.2 weight part are added in the still; Be heated to the 110-120 degree; Vacuum-drying 2 hours; Nitrogen protection adds skimmer 5,500 0.5 weight parts down, mixes the nitrogen protection bottom discharge.
Second component: MDI-50 is with respect to first component 65 weight parts
First and second components are mixed back (vacuum defoamation in case of necessity) with the weight ratio of 100:65 make sample to be tested.
Embodiment 4
First component: Viscotrol C 61 weight parts, fire retardant FR-600 36 weight part, inferior tin 0.1 weight part of octoate catalyst, antioxidant 1010 0.2 weight part, UV light absorber UV-327 0.2 weight part are added in the still; Be heated to the 110-120 degree; Vacuum-drying 2 hours; Nitrogen protection adds skimmer 5,500 0.5 weight parts down, mixes the nitrogen protection bottom discharge.
The second component: poly methylene poly phenyl poly isocyanate is with respect to first component 65 weight parts
First and second components are mixed back (vacuum defoamation in case of necessity) with the weight ratio of 100:65 make sample to be tested.
The comparative example 1
First component: hydroxy-terminated polybutadienes (molecular weight 2500-3500) 62 weight parts, fire retardant FR-lm6 37 weight parts, catalyzer dibutyl tin laurate 0.1 weight part, antioxidant 1010 0.2 weight part, UV light absorber UV-327 0.2 weight part are added in the still; Be heated to the 110-120 degree; Vacuum-drying 2 hours; Nitrogen protection adds skimmer 5,500 0.5 weight parts down, mixes the nitrogen protection bottom discharge.
Second component: MDI-50 is with respect to first component 6.5 weight parts.
First and second components are mixed back (vacuum defoamation in case of necessity) with the weight ratio of 100:6.5 make sample to be tested.
The comparative example 2
First component: Viscotrol C 99 weight parts, catalyzer dibutyl tin laurate 0.1 weight part, antioxidant 1010 0.2 weight part, UV light absorber UV-327 0.2 weight part are added in the still; Be heated to the 110-120 degree; Vacuum-drying 2 hours; Nitrogen protection adds non-silicone high molecular polymer skimmer 0.5 weight part down, mixes the nitrogen protection bottom discharge.
Second component: MDI-50 is with respect to first component 40 weight parts
A, B component are mixed back (vacuum defoamation in case of necessity) with the weight ratio of 100:40 make test specimen to be measured.
Test example 1 viscosity test
The foregoing description 1-3 and comparative example 1 are detected according to GB/T 2794-1995
The test of test example 2 gel times
The foregoing description 1-3 and comparative example 1 are tested according to standard GB 12007.7-89.
Test example 3 tensile strengths and elongation at break test
The foregoing description 1-3 and comparative example 1 are tested according to standard GB/T 528-1998
The test of test example 4 flame retardant ratings
The foregoing description 1-3 and comparative example 1 are tested according to standard UL 94
Test gained result is shown in table one.
Table one test gained result
Can find out that from the result of last table one though comparative example 1 has reached fire-retardant requirement, its price is high, and viscosity is high.Embodiment 1-4 does not add softening agent, has reached low viscous requirement yet.Contrast does not add the comparative example 2 of reactive flame retardant; The operating procedure of product and product performance change little; But flame retardant rating but is greatly improved, and in the embodiment 1-4, along with the raising of reactive flame retardant phosphorus content in the prescription; Flame retardant rating also improving, has satisfied fire-retardant needs.
The above is merely preferred embodiment of the present invention, and is in order to restriction the present invention, not all within spirit of the present invention and principle, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a flame retardant polyurethane pouring sealant is characterized in that, is that the first component and the second component of 100:60～65 formed by weight proportion; Said first component is made up of the raw material of following parts by weight: 60 parts～75 parts oligomer polyol, 0.1 part catalyzer, 0.4 part stablizer, 0.5 part skimmer, 24 parts～39 parts liquid flame retardant; Wherein, Said oligomer polyol is a Viscotrol C, and said liquid flame retardant is that Qingdao joins phosphorous, nitrogen reactive-type flame retardant FR-lm6 or the FR-600 beautify the worker; Said second component is an isocyanic ester; Said isocyanic ester comprises 2; 4-diphenylmethanediisocyanate and 4, a kind of or any several kinds mixture in 4 '-mixtures of diisocyanates and diphenylmethane, poly methylene poly phenyl poly isocyanate, liquefied mdi and the isophorone diisocyanate.
2. flame retardant polyurethane pouring sealant according to claim 1 is characterized in that, said catalyzer comprises a kind of or any several kinds mixture in dibutyl tin laurate, stannous octoate, three Bismuth Octoates and three bismuth valerates.
3. flame retardant polyurethane pouring sealant according to claim 1 is characterized in that, said stablizer is antioxidant 1010 and UV light absorber UV-327.
4. flame retardant polyurethane pouring sealant according to claim 1 is characterized in that, said skimmer is a kind of or any several kinds mixture that comprises in non-silicone high molecular polymer, modified polyorganosiloxane and the acrylic ester copolymerization thing.
5. the preparation method of a flame retardant polyurethane pouring sealant is characterized in that, said preparation method comprises: at first, make first component and second component; Then; Is that 100:60～65 mix and get final product with first component and second component according to weight proportion; The preparation of said first component comprises oligomer polyol, catalyzer, stablizer, skimmer and liquid flame retardant is joined in the reaction kettle; Heat while stirring, be heated to 110 ℃～120 ℃ under vacuum condition dry 2 hours, again under protection of nitrogen gas after the cooling; Pack and get final product, the preparation of said second component comprises isocyanic ester mixed directly to pack under protection of nitrogen gas and gets final product; Wherein, Said first component is made up of the raw material of following parts by weight: 60 parts～75 parts oligomer polyol, 0.1 part catalyzer, 0.4 part stablizer, 0.5 part skimmer, 24 parts～39 parts liquid flame retardant; Said oligomer polyol is a Viscotrol C, and said liquid flame retardant is that Qingdao joins phosphorous, nitrogen reactive-type flame retardant FR-lm6 or the FR-600 beautify the worker; Said isocyanic ester comprises 2,4-diphenylmethanediisocyanate and 4, a kind of or any several kinds mixture in 4 '-mixtures of diisocyanates and diphenylmethane, poly methylene poly phenyl poly isocyanate, liquefied mdi and the isophorone diisocyanate.
6. the method for use of a flame retardant polyurethane pouring sealant is characterized in that, said method of use comprises: at first, will treat that the embedding part carries out drying treatment; Then, flame retardant polyurethane pouring sealant as claimed in claim 1 is poured into treats on the embedding part, at room temperature solidifying 24 hours or being heating and curing and gets final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010278348 CN101928377B (en) | 2010-09-10 | 2010-09-10 | Flame retardant polyurethane pouring sealant, preparation method thereof and using method thereof |
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| CN 201010278348 CN101928377B (en) | 2010-09-10 | 2010-09-10 | Flame retardant polyurethane pouring sealant, preparation method thereof and using method thereof |
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| CN101928377B true CN101928377B (en) | 2012-12-19 |
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| CN111808570A (en) * | 2020-08-27 | 2020-10-23 | 格丽泰新材料科技（苏州）有限公司 | Double-component polyurethane adhesive and application thereof |
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| CN101096583A (en) * | 2006-06-26 | 2008-01-02 | 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101096583A (en) * | 2006-06-26 | 2008-01-02 | 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111808570A (en) * | 2020-08-27 | 2020-10-23 | 格丽泰新材料科技（苏州）有限公司 | Double-component polyurethane adhesive and application thereof |
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