CN102627937A - Bi-component conductive polyurethane pouring adhesive and preparation method thereof - Google Patents
Bi-component conductive polyurethane pouring adhesive and preparation method thereof Download PDFInfo
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- CN102627937A CN102627937A CN2012100843802A CN201210084380A CN102627937A CN 102627937 A CN102627937 A CN 102627937A CN 2012100843802 A CN2012100843802 A CN 2012100843802A CN 201210084380 A CN201210084380 A CN 201210084380A CN 102627937 A CN102627937 A CN 102627937A
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Abstract
The invention discloses a bi-component conductive polyurethane pouring adhesive and a preparation method thereof, wherein a component I is obtained by evenly mixing polymer polyol, chain extenders, catalytic agents, antifoaming agents and modified thermal fillers, and a component II is isocyanate. When in specific use, the two components are evenly mixed and solidified after pouring. The pouring adhesive is free of solvent, environment-friendly, moderate in viscosity and capable of being solidified at the normal temperature or rising temperature, and has the advantages of being good in insulation, flexibility, adhesion and low-temperature performance, capable of being used in a wide temperature range and the like, and has the conductive factor as high as 1.5W/m*K.
Description
One, technical field
The present invention relates to a kind of joint sealant and preparation method thereof, specifically a kind of two-pack heat-conduction polyurethane joint sealant and preparation method thereof.
Two, background technology
As everyone knows, along with science and technology development, the kind of electronic devices and components is more and more, and the connection of circuit is subtilizedization and densification also, thereby the stability of each assembly of electron device has been proposed very big requirement.In order to prevent that moisture, dust etc. from getting into electron device, make electronic devices and components more stable, need carry out embedding to electron device.Embedding can avoid electron device to be directly exposed in the air, has intercepted that the direct of acid-base material contacts in electron device and water and the air, simultaneously electron device is combined, and has guaranteed the globality of electron device, has improved the stability of electron device.Polyurethane pouring sealant has preferably water resistance, good insulation preformance, hardness can be in harmonious proportion adhesive property preferably; Can improve the resistibility of device to external shock and vibrations; Avoid components and parts, circuit to be directly exposed in the air, improve waterproof, the Corrosion Protection of electron device.But electron device can produce a large amount of heat in the course of the work, if can not in time distribute, will cause the components and parts short circuit, situation such as burns, and this has just proposed very high requirement to the heat conductivility of joint sealant.In addition, most of polyurethane pouring sealant contains softening agent, does not meet environmental protection requirement, and the insulativity of joint sealant is relatively poor, does not meet the insulating requirements of electronic devices and components.At present both at home and abroad more to the research of heat conduction organosilicon filling and sealing gum, and to the research of urethane heat conduction joint sealant seldom and heat-conducting effect not ideal.
Three, summary of the invention
The present invention aims to provide a kind of two-pack heat-conduction polyurethane joint sealant and preparation method thereof, and technical problem to be solved is to give the polyurethane pouring sealant heat conductivility, thereby solves the heat dissipation problem after the electron device embedding.
Technical solution problem of the present invention adopts following technical scheme:
The raw material of two-pack heat-conduction polyurethane joint sealant of the present invention constitutes by mass fraction:
Component A: polymer polyatomic alcohol 30-60 part, chainextender 1-3 part, catalyzer 0.5-2 part, skimmer 0.5-2 part, modification heat conductive filler 120-250 part;
B component: isocyanic ester;
The ratio of the quality of component A and component B is 100: 5-20;
In the raw material:
Said polymer polyatomic alcohol is selected from Viscotrol C or polyether glycol;
Said chainextender is selected from alcohol compound or aminated compounds; Said alcohol compound is selected from 1,4-butyleneglycol, USP Kosher, terepthaloyl moietie, 1, ammediol, TriMethylolPropane(TMP) (TMP), 1, one or more in 6-pinakon, two (beta-hydroxyethyl) ethers (HQEE) of Resorcinol; Said aminated compounds is selected from 3,3 '-dichloro-4,4,4 '-ditan diamines (MOCA), 3; 5-diformazan sulfenyl tolylene diamine (DMTDA), 3; 5-diethyl toluene diamine (DETDA), 2,4-diamino--3, one or more in the 5-diformazan sulfenyl chlorobenzene (TX-2);
Said catalyzer is selected from amines catalyst, organic tin catalyzer or titanate ester catalyzer;
Said skimmer is selected from one or more in polyoxyethylene polyoxypropylene tetramethylolmethane ether, methyl-silicone oil, T 46155 polyoxy propyl alcohol amidogen ether, the polyoxypropylene glyceryl ether;
Said modification heat conductive filler carries out obtaining after the surface modification treatment to heat conductive filler with surface-modifying agent, and the addition of surface-modifying agent is the 0.5-5% of heat conductive filler quality; Wherein surface-modifying agent is selected from one or more in 3-aminopropyl oxyethyl group siloxanes (KH550), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), γ-(methacryloxypropyl) propyl trimethoxy silicane (KH570), dodecyl Trimethoxy silane, vinyltriethoxysilane, the titanic acid ester; Heat conductive filler is selected from aluminum oxide (Al
2O
3), in the zinc oxide (ZnO), aluminium nitride AlN (AlN), SP 1 (BN), thomel, spun glass one or more;
Said isocyanic ester is selected from HDI (HDI), tetramethyl-benzene dimethyl-vulcabond (TMXDI), diphenylmethanediisocyanate (MDI), isophorone diisocyanate (IPDI), 2; 4 or 2, one or more in 6-tolylene diisocyanate (TDI), the poly methylene poly phenyl poly isocyanate.
Said polyether glycol is selected from one or more in polyether Glycols, polyether-tribasic alcohol, the polyethers tetravalent alcohol, and the number-average molecular weight of said polyether glycol is 600-3000.
In the preferred fluorochemical polyether divalent alcohol of said polyether glycol, polyoxypropyleneglycol, polyoxytrimethylene triol, the polyoxytrimethylene tetrol one or more, number-average molecular weight is 600-3000.
Said amines catalyst is selected from triethylenediamine, N, N, N '; N '-tetramethylene Alkylenediamine, N; N-dimethyl-Bian amine, N, N, the two aminoethyl ethers of N '-trimethylammonium-N '-hydroxyethyl, N; N '-2-N-METHYL PIPERAZINE, N-2-hydroxypropyl thebaine, N, one or more in N-dimethylethanolamine, the trolamine.
Said organic tin catalyzer is selected from one or more in dibutyl tin laurate (DBTDL), stannous octoate, two (dodecyl sulphur) dibutyl tin, the dibutyltin diacetate.
Said titanate ester catalyzer is selected from titanium isopropylate and/or tetrabutyl titanate.
The preparation method of two-pack heat-conduction polyurethane joint sealant of the present invention comprises the preparation of component I and component I I:
The preparation of said component I is that each raw materials mix among the component A is evenly got final product, and wherein polymer polyatomic alcohol is handled 100-120 ℃ of vacuum hydro-extraction in advance, and the modification heat conductive filler is in advance 90-100 ℃ of drying treatment;
The preparation of said component I I is that the raw material with B component mixes to pack under nitrogen protection and gets final product.
Concrete encapsulating method:
During embedding component I and component I I mixed by proportional quantity and obtain joint sealant, joint sealant is poured on the device that needs embedding, under the condition of vacuum normal temperature Procuring 5-12 hour, solidify in 60-80 ℃ again and got final product in 5-10 hour.
Modification heat conductive filler of the present invention prepares by following method:
In the surface-modifying agent of 10-100g, add the absolute ethyl alcohol of 20-200g and the deionized water of 3-20g, mix with the 2000g heat conductive filler behind the hydrolysis 20-30min, in high-speed mixer, get final product in 100-120 ℃ of reaction 10-30min.
Joint sealant thermal conductivity of the present invention is high, solidifies the no bubble in back, and surface drying time can be adjusted; Operable time is long, and is strong to glass, metal sticking effect, the separately sealing of A, B component; The good stability of joint sealant, the storage time is long, and is all curable under normal temperature and comparatively high temps; Easy to use, viscosity can be adjusted, applicable to the embedding of multiple electron device.
Four, embodiment
Embodiment 1:
1, component I:
With 40g polyoxytrimethylene divalent alcohol (Mn=1000) in 120 ℃ of following vacuum hydro-extraction 4h; Be cooled to the aluminum oxide of the dibutyl tin laurate that adds 2g USP Kosher, 0.5g after the room temperature, 0.5g stannous octoate, 2g methyl-silicone oil, 120g KH550 modification; High-speed stirring 0.5h makes component I on impeller;
2, component I I:
The liquefied mdi of weighing 16g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 10 hours under the condition of vacuum normal temperature, solidifies in 70 ℃ to get final product in 10 hours again.
Comparative Examples 1:
The preparation method of this Comparative Examples is with embodiment 1, and different is not add heat conductive filler.
Embodiment 2:
1, component I:
With 60g polyoxytrimethylene trivalent alcohol (Mn=600) in 120 ℃ of following vacuum hydro-extraction 4h; Add 1.5g1 after being cooled to room temperature; The aluminum oxide of the dibutyl tin laurate of ammediol, 1g, 2g methyl-silicone oil, the modification of 400g tetrabutyl titanate; High-speed stirring 1.5h makes component I on impeller;
2, component I I:
The isophorone diisocyanate of weighing 25g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 5 hours under the condition of vacuum normal temperature, solidifies in 65 ℃ to get final product in 10 hours again.
Comparative Examples 2:
The preparation method of this Comparative Examples is with embodiment 2, and different is the heat conductive filler surface-modifying agent modification of no use that adds.
Embodiment 3:
1, component I:
With 60g polyoxytrimethylene divalent alcohol (Mn=1500) in 120 ℃ of following vacuum hydro-extraction 4h; Be cooled to stannous octoate, the 2g methyl-silicone oil of the dibutyl tin laurate that adds 2g TriMethylolPropane(TMP) (TMP), 0.5g after the room temperature, 1g, the aluminium nitride AlN of 140g tetrabutyl titanate modification; High-speed stirring 1h makes component I on impeller;
2, component I I:
The isophorone diisocyanate of weighing 15g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 7 hours under the condition of vacuum normal temperature, solidifies in 80 ℃ to get final product in 5 hours again.
Embodiment 4:
1, component I:
With 40g polyoxytrimethylene divalent alcohol (Mn=1000) and 20g Viscotrol C (Mn=930) in 120 ℃ of following vacuum hydro-extraction 4h; Be cooled to the aluminum oxide of the dibutyl tin laurate that adds 2g terepthaloyl moietie, 1g after the room temperature, 2g methyl-silicone oil, the modification of 240g tetrabutyl titanate; High-speed stirring 0.5h makes component I on impeller;
2, component I I:
The isophorone diisocyanate of weighing 28g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 10 hours under the condition of vacuum normal temperature, solidifies in 75 ℃ to get final product in 8 hours again.
Embodiment 5:
1, component I:
With 50g Viscotrol C (Mn=930) in 120 ℃ of following vacuum hydro-extraction 4h; Add 0.5g1 after being cooled to room temperature; The aluminium nitride AlN of the triethylenediamine of 4-butyleneglycol, 1g, 2g polyoxypropylene glyceryl ether, the modification of 320g dodecyl Trimethoxy silane and the ZnO of 20g dodecyl Trimethoxy silane modification; High-speed stirring 1.5h makes component I on impeller;
2, component I I:
The HDI of weighing 26g (is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 10 hours under the condition of vacuum normal temperature, solidifies in 65 ℃ to get final product in 8 hours again.
Embodiment 6:
1, component I:
With 40g polyoxytrimethylene trivalent alcohol (Mn=600) and 20g Viscotrol C (Mn=930) in 120 ℃ of following vacuum hydro-extraction 4h; Be cooled to the N that adds 0.5g TriMethylolPropane(TMP), 0.5g after the room temperature; The aluminum oxide of the stannous octoate of N-dimethylethanolamine and 0.5g, 1.5g T 46155 polyoxy propyl alcohol amidogen ether, the modification of 150g titanic acid ester; High-speed stirring 0.5h makes component I on impeller;
2, component I I:
The TDI of weighing 27g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 5 hours under the condition of vacuum normal temperature, solidifies in 80 ℃ to get final product in 10 hours again.
Embodiment 7:
1, component I:
With 60g polyoxytrimethylene tetravalent alcohol (Mn=3740) in 120 ℃ of following vacuum hydro-extraction 4h; Add 1.5g1 after being cooled to room temperature; The ZnO of the aluminum oxide of the trolamine of 4-butyleneglycol, 0.5g, 2g methyl-silicone oil, the modification of 120g vinyltriethoxysilane and the modification of 12g dodecyl Trimethoxy silane; High-speed stirring 1h makes component I on impeller;
2, component I I:
The isophorone diisocyanate of weighing 28g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 12 hours under the condition of vacuum normal temperature, solidifies in 75 ℃ to get final product in 5 hours again.
Embodiment 8:
1, component I:
With 40g polyoxytrimethylene divalent alcohol (Mn=1500) and 20g Viscotrol C (Mn=930) in 120 ℃ of following vacuum hydro-extraction 4h; Add 0.5g3 after being cooled to room temperature; 3 '-dichloro-4,4; 4 '-aluminium nitride AlN of the dibutyltin diacetate of ditan diamines, 1g, 2g methyl-silicone oil, 300g KH560 modification, high-speed stirring 1.5h makes component I on impeller;
2, component I I:
The liquefied mdi of weighing 23g is component I I;
During embedding component I and component I I mixed and obtain joint sealant, joint sealant is poured on the device that needs embedding, Procuring is 12 hours under the condition of vacuum normal temperature, solidifies in 65 ℃ to get final product in 8 hours again.
The performance test of joint sealant:
Mixing viscosity tests according to GB/T 2794-1995.
Tensile strength, elongation are tested according to GB/T16777-2008.
Thermal conductivity is tested according to GB/T3399-1982.
From table, can find out that the adding of heat conductive filler makes the thermal conductivity of urethane that very big raising arranged, along with the increasing of heat conductive filler amount, the thermal conductivity of urethane increases gradually.The adding of filler has certain strengthening action to matrix.Use the heat conductive filler of surface-modifying agent modification bigger to the raising of matrix thermal conductivity than the heat conductive filler that does not have modification.
Claims (7)
1. two-pack heat-conduction polyurethane joint sealant is characterized in that its raw material constitutes by mass fraction:
Component A: polymer polyatomic alcohol 30-60 part, chainextender 1-3 part, catalyzer 0.5-2 part, skimmer 0.5-2 part, modification heat conductive filler 120-250 part;
B component: isocyanic ester;
The ratio of the quality of component A and component B is 100: 5-20;
In the raw material:
Said polymer polyatomic alcohol is selected from Viscotrol C or polyether glycol;
Said chainextender is selected from alcohol compound or aminated compounds; Said alcohol compound is selected from 1,4-butyleneglycol, USP Kosher, terepthaloyl moietie, 1, ammediol, TriMethylolPropane(TMP), 1, one or more in 6-pinakon, two (beta-hydroxyethyl) ethers of Resorcinol; Said aminated compounds is selected from 3,3 '-dichloro-4,4,4 '-ditan diamines, 3,5-diformazan sulfenyl tolylene diamine, 3,5-diethyl toluene diamine, 2,4-diamino--3, one or more in the 5-diformazan sulfenyl chlorobenzene;
Said catalyzer is selected from amines catalyst, organic tin catalyzer or titanate ester catalyzer;
Said skimmer is selected from one or more in polyoxyethylene polyoxypropylene tetramethylolmethane ether, methyl-silicone oil, T 46155 polyoxy propyl alcohol amidogen ether, the polyoxypropylene glyceryl ether;
Said modification heat conductive filler carries out obtaining after the surface modification treatment to heat conductive filler with surface-modifying agent; Wherein surface-modifying agent is selected from one or more in 3-aminopropyl oxyethyl group siloxanes, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, dodecyl Trimethoxy silane, vinyltriethoxysilane, the titanic acid ester; Heat conductive filler is selected from one or more in aluminum oxide, zinc oxide, aluminium nitride AlN, SP 1, thomel, the spun glass;
Said isocyanic ester is selected from HDI, tetramethyl-benzene dimethyl-vulcabond, diphenylmethanediisocyanate, isophorone diisocyanate, 2; 4 or 2, one or more in 6-tolylene diisocyanate, the poly methylene poly phenyl poly isocyanate.
2. two-pack heat-conduction polyurethane joint sealant according to claim 1; It is characterized in that: said polyether glycol is selected from one or more in polyether Glycols, polyether-tribasic alcohol, the polyethers tetravalent alcohol, and the number-average molecular weight of said polyether glycol is 600-3000.
3. two-pack heat-conduction polyurethane joint sealant according to claim 1 and 2 is characterized in that: said polyether glycol is selected from one or more in fluorochemical polyether divalent alcohol, polyoxypropyleneglycol, polyoxytrimethylene triol, the polyoxytrimethylene tetrol.
4. two-pack heat-conduction polyurethane joint sealant according to claim 1, it is characterized in that: said amines catalyst is selected from triethylenediamine, N, N; N ', N '-tetramethylene Alkylenediamine, N, N-dimethyl-Bian amine, N; N; The two aminoethyl ethers of N '-trimethylammonium-N '-hydroxyethyl, N, N '-2-N-METHYL PIPERAZINE, N-2-hydroxypropyl thebaine, N, one or more in N-dimethylethanolamine, the trolamine.
5. two-pack heat-conduction polyurethane joint sealant according to claim 1 is characterized in that: said organic tin catalyzer is selected from one or more in dibutyl tin laurate, stannous octoate, two (dodecyl sulphur) dibutyl tin, the dibutyltin diacetate.
6. two-pack heat-conduction polyurethane joint sealant according to claim 1 is characterized in that: said titanate ester catalyzer is selected from titanium isopropylate and/or tetrabutyl titanate.
7. the preparation method of the described two-pack heat-conduction polyurethane of claim 1 joint sealant comprises the preparation of component I and component I I, it is characterized in that:
The preparation of said component I is that each raw materials mix among the component A is evenly got final product, and wherein polymer polyatomic alcohol is handled 100-120 ℃ of vacuum hydro-extraction in advance, and the modification heat conductive filler is in advance 90-100 ℃ of drying treatment;
The preparation of said component I I is that the raw material with B component mixes to pack under nitrogen protection and gets final product.
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