CN105255111B - A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material - Google Patents

A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material Download PDF

Info

Publication number
CN105255111B
CN105255111B CN201510704833.0A CN201510704833A CN105255111B CN 105255111 B CN105255111 B CN 105255111B CN 201510704833 A CN201510704833 A CN 201510704833A CN 105255111 B CN105255111 B CN 105255111B
Authority
CN
China
Prior art keywords
filler
modified
thermal conductivity
encapsulation material
coupling agent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510704833.0A
Other languages
Chinese (zh)
Other versions
CN105255111A (en
Inventor
谭育新
陈军
揭春龙
杨安学
陈贵立
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangzhou xinlaifu New Material Co.,Ltd.
Original Assignee
Guangzhou Newlife Magnet Electricity Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangzhou Newlife Magnet Electricity Co Ltd filed Critical Guangzhou Newlife Magnet Electricity Co Ltd
Priority to CN201510704833.0A priority Critical patent/CN105255111B/en
Publication of CN105255111A publication Critical patent/CN105255111A/en
Application granted granted Critical
Publication of CN105255111B publication Critical patent/CN105255111B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Compositions Of Macromolecular Compounds (AREA)
  • Epoxy Resins (AREA)
  • Thermistors And Varistors (AREA)

Abstract

The invention discloses a kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material, preparation includes step:1)First inorganic nano-filler, isocyanates, catalyst are fully reacted, the filler of isocyanate-modified is prepared;2)The filler of isocyanate-modified, hyper-branched polyester, catalyst are fully reacted, modified filler 1 is prepared;3)Second inorganic nano-filler, coupling agent are fully reacted, the filler of coupling agent modification is obtained;4)The filler of coupling agent modification, activated monomer, catalyst are fully reacted, modified filler 2 is obtained;5)Modified filler 1 and modified filler 2 are disperseed in the epoxy.Also disclose that application of the epoxide resin encapsulation material of above method preparation in high thermal conductivity coefficient thermistor is prepared.After hardening, gained solidfied material has thermal conductivity factor very high to epoxide resin encapsulation material prepared by the present invention, for the NTC thermistor of existing structure in, can be with the reaction speed of larger quickening sensor.

Description

A kind of preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material and Using
Technical field
The present invention relates to a kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material.
Background technology
Negative temperature coefficient(NTC)Thermistor refers to the electron ceramic material that resistance is raised and declined with temperature.In refrigerator, In the field of household appliances such as water heater, coffee machine, measurement temperature is used for through the thermistor frequently with resin embedding type.With market and The demand for development more and more higher of technology, the reaction speed of NTC temperature sensors needs as much as possible soon, and this is just to the ring of encapsulation The thermal conductivity factor of oxygen tree fat proposes requirement higher.
Existing thermistor embedding epoxy resin substantially on solve unborn poor insulativity, being bonded and sealed property is not The problems such as good and not impact resistance, but to thermal conductivity factor, this performance is all paid little attention to, therefore thermal conductivity factor is not high, often only There is 0.2 ~ 0.5 Wm-1K-1Left and right, it is impossible to meet to the highly sensitive requirement of temperature sensing.It is common to do to improve thermal conductivity factor Method is to adding inorganic filler in epoxy resin, but generally to need the loading higher could to form effective heat conduction network, from And cause the follow-up inconvenient using technological operation of epoxy resin.In addition, if heat conducting nano powder is directly added, but due to receiving Ground rice body surface in itself can be high, is difficult to be uniformly dispersed in resin matrix, so as to greatly suppress carrying for resin heat conductivility Rise.
The content of the invention
It is an object of the invention to provide a kind of preparation side of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material Method and application.
The technical solution used in the present invention is:
The preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material, comprises the following steps:
1)The moditied processing of the first inorganic nano-filler:First inorganic nano-filler, isocyanates, catalyst have been mixed in In machine solvent, fully reaction, separation of solid and liquid, gained solid is fully dried, and grinding obtains the filler of isocyanate-modified;
2)The filler of isocyanate-modified, hyper-branched polyester, catalyst are placed in organic solvent, under protective atmosphere, Fully reaction, products therefrom is separated, and is washed, and is fully dried, and obtains modified filler 1;
3)The moditied processing of the second inorganic nano-filler:Second inorganic nano-filler, coupling agent are mixed in organic solvent, Fully reaction, isolates product, obtains the filler of coupling agent modification;
4)Filler, activated monomer, the catalyst mixing that coupling agent is modified, under protective atmosphere, are fully reacted, and are separated Go out product, wash, dry, obtain modified filler 2;
5)Modified filler 1 and modified filler 2 is dispersed in the epoxy.
Described the first inorganic nano-filler, the second inorganic nano-filler are independently selected from following inorganic nano-filler In at least one:BN、Al2O3、AlN、BN、MgO、ZnO、SiO2、Si3N4, SiC, BeO, carbon dust, Graphene, graphite powder.
Described isocyanates is in MDI, HDI, NDI, PPDI, IPDI, XDI, TDI, PAPI, HTDI, HMDI, CHDI It is at least one.
Described hyper-branched polyester be Boltorn H20, Boltorn H30, Boltorn H40, Boltorn U3000, At least one in Boltorn W3000, Boltorn H2004.
Described coupling agent be silane coupler, titanate coupling agent, aluminate coupling agent, zirconium ester coupling agent in extremely Few one kind.
Described activated monomer is N, N- dihydroxy ethyl -3- amido methyl propionates.
Step 1)In, the first inorganic nano-filler, the mass ratio of isocyanates are(5-20):1.
Step 2)In, the filler of isocyanate-modified, the amount ratio of hyper-branched polyester are:1g:(2-10)mL.
Step 3)In, the mass ratio of the second inorganic nano-filler and coupling agent is(1-20):1;Step 4)In, coupling agent is repaiied The filler of decorations, the amount ratio of activated monomer are(5-20)g:1mol.
Application of the epoxide resin encapsulation material of above-mentioned preparation in high thermal conductivity coefficient thermistor is prepared.
The beneficial effects of the invention are as follows:
After hardening, gained solidfied material has thermal conductivity factor very high to epoxide resin encapsulation material prepared by the present invention, uses In the NTC thermistor of existing structure, can be with the reaction speed of larger quickening sensor.
Specific embodiment
The preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material, comprises the following steps:
1)The moditied processing of the first inorganic nano-filler:First inorganic nano-filler, isocyanates, catalyst have been mixed in In machine solvent, fully reaction, separation of solid and liquid, gained solid is fully dried, and grinding obtains the filler of isocyanate-modified;
2)The filler of isocyanate-modified, hyper-branched polyester, catalyst are placed in organic solvent, under protective atmosphere, Fully reaction, products therefrom is separated, and is washed, and is fully dried, and obtains modified filler 1;
3)The moditied processing of the second inorganic nano-filler:Second inorganic nano-filler, coupling agent are mixed in organic solvent, Fully reaction, separation of solid and liquid, be dried to obtain coupling agent modification filler;
4)Filler, activated monomer, the catalyst mixing that coupling agent is modified, under protective atmosphere, are fully reacted, and are separated Go out product, wash, dry, obtain modified filler 2;
5)Modified filler 1 and modified filler 2 is dispersed in the epoxy.
Preferably, the first described inorganic nano-filler, the second inorganic nano-filler are independently selected from following inorganic At least one in Nano filling:BN、Al2O3、AlN、BN、MgO、ZnO、SiO2、Si3N4, SiC, BeO, carbon dust, Graphene, stone Ink powder;
Preferably, step 1)In, described catalyst is organotin catalysts;It is further preferred that being tin dilaurate two Butyl tin, stannous octoate, two (dodecyl sulphur) dibutyl tins, dibutyltin diacetate, tin dilaurate dioctyl tin, dialkyl group At least one in tin dimaleate, two mercaptan tin alkyls;Still more preferably, it is dibutyl tin laurate;
Preferably, step 1)In, described isocyanates is MDI, HDI, NDI, PPDI, IPDI, XDI, TDI, PAPI, At least one in HTDI, HMDI, CHDI;
Preferably, step 1)In, the first inorganic nano-filler, the mass ratio of isocyanates are(5-20):1;
Preferably, step 1)In, reaction is carried out in microwave reactor, and the condition of reaction is:Temperature:40-120 ℃;Time:20-60min;Stir speed (S.S.):300-500rpm;
Preferably, step 2)In, described hyper-branched polyester is Boltorn H20, Boltorn H30, Boltorn At least one in H40, Boltorn U3000, Boltorn W3000, Boltorn H2004;It is further preferred that being Boltorn H20;
Preferably, step 2)In, described protective atmosphere is selected from least one in nitrogen, helium, argon gas, neon;Enter One step is preferred, is at least one in nitrogen, argon gas;
Preferably, step 2)In, described catalyst is organotin catalysts;It is further preferred that being tin dilaurate two Butyl tin, stannous octoate, two (dodecyl sulphur) dibutyl tins, dibutyltin diacetate, tin dilaurate dioctyl tin, dialkyl group At least one in tin dimaleate, two mercaptan tin alkyls;Still more preferably, it is dibutyl tin laurate;
Preferably, step 2)In, the filler of isocyanate-modified, the amount ratio of hyper-branched polyester are:1g:(2-10)mL;
Preferably, step 2)In, reaction is carried out in microwave reactor, and the condition of reaction is:Temperature:40-120 ℃;Time:10-20h;Stir speed (S.S.):300-500rpm;
Preferably, step 3)In, described coupling agent is silane coupler, titanate coupling agent, aluminate coupling agent, zirconium At least one in acid esters coupling agent;It is further preferred that described coupling agent is silane coupler;Still more preferably, The formula of silane coupler is:YSiX3;In formula, Y is non-hydrolytic group, selected from the one kind in following group:Alkenyl, alkyl, Alkyl of the end with following at least one functional group:Cl、NH2, SH, epoxy, N3、(Methyl)Acryloxy, isocyanates Base, i.e. Y are carbon functional group;X is hydrolyzable groups, selected from the one kind in following groups:Cl、OMe、 OEt、 OC2H4OCH3、 OSiMe3、OAc;For example silane coupler can be:In KH550, KH560, KH570, KH792, KH580, KH602, A171 extremely Few one kind;
Preferably, step 3)In, the mass ratio of the second inorganic nano-filler and coupling agent is(1-20):1;
Preferably, step 3)Carried out in microwave reactor, the condition of reaction is:Reaction temperature:40-120 DEG C, instead Between seasonable:10-60min;Stir speed (S.S.):300-500rpm;
Preferably, step 1)-3)In, described organic solvent is polar organic solvent or aromatic hydrocarbon solvent, such as halo Hydro carbons, esters, ethers, organic acid, alcohols, alcohol ethers, amine, oxygen heterocycle, containing in S, solvent containing P, benzene series solvent extremely Few one kind;Specifically, for example:In ethyl acetate, glycol monoethyl ether, dioxane, chloroform, toluene, benzene, dimethylbenzene at least It is a kind of.
Preferably, step 4)In, described activated monomer is N, N- dihydroxy ethyl -3- amido methyl propionates.
Preferably, step 4)In, described catalyst is acid catalyst, it is further preferred that for the concentrated sulfuric acid, to toluene At least one in sulfonic acid, solid super-strong acid, DBSA;Still more preferably, it is p-methyl benzenesulfonic acid;
Preferably, step 4)In, described protective atmosphere is selected from least one in nitrogen, helium, argon gas, neon;Enter One step is preferred, is at least one in nitrogen, argon gas;
Preferably, step 4)In, the filler of coupling agent modification, the amount ratio of activated monomer are(5-20)g:1mol;
Preferably, step 4)In, reaction is carried out in microwave reactor;The condition of reaction is:Reaction temperature:100- 150℃;Reaction time:2-10h;Stir speed (S.S.):300-500rpm;
Preferably, step 5)In, the mass ratio of modified filler 1 and modified filler 2 is any, and modified filler 1 is filled out with modified The gross mass of material 2 is the 10-30wt% of epoxy resin;
Preferably, step 5)In, first modified filler 1 and modified filler 2 are well mixed, then be dispersed in epoxy resin In;Modified filler 1 and the mode of the mixing of modified filler 2 are:Both are mixed in organic solvent, then ball milling is uniformly dispersed;Change Property uniform filling dispersion mode in the epoxy be:Carry out being sufficiently mixed dispersion in microwave reactor, mix scattered Temperature is:100-150℃;Mixing the scattered time is:60-150min;Mixing stir speed (S.S.) when disperseing is:300- 500rpm;
Preferably, step 5)In, described epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol S At least one in type epoxy resin, bisphenol-A D-ring oxygen tree fat;It is further preferred that being bisphenol A type epoxy resin;
Preferably, application of the epoxide resin encapsulation material of above-mentioned preparation in high thermal conductivity coefficient thermistor is prepared;
In the present invention, high thermal conductivity coefficient refers to thermal conductivity factor >=1 Wm-1K-1;Further, it is 1-2.5 Wm-1K-1
With reference to specific embodiment, the present invention is described further:
It should be noted that:In the present invention, tested used by " bullet-shaped thermistor " for prior art product Described in product, such as patent 201210181643.1.
Embodiment 1:
1. the processing procedure of nanometer BN:10g nanometers of BN is weighed, 400ml anhydrous dioxanes surpass in the flask of 2500ml Dispersion 30min is swung in acoustic shock, then by BN and hexamethylene diisocyanate(HDI)Mass ratio is 6:1 ratio adds six methylenes Group diisocyanate and 0.5ml catalyst dibutyltin cinnamic acid dibutyl alkene(DBTDL), the speed of 400rpm is pressed in microwave reactor Stirring, 40 ~ 120 DEG C of 20 ~ 60min of reaction, cooling room temperature filtering, high speed centrifugation removes unnecessary HDI, and through drying, milling obtains Through the BN-M that HDI is modified.
Weigh above-mentioned BN-M10g, hyper-branched polyester H20 38.5g(23.8ml)With 1000ml anhydrous dioxanes, together It is added in flask, is passed through argon gas protection, add the DBTDL of 0. 5ml, is stirred by the speed of 400rpm in microwave reactor Mix, 75 DEG C of reaction 12h, just resulting polymers are vacuum dried 4h in 80 DEG C after removing unnecessary H20 and washes clean, are surpassed The modified nanometer BN of branched polyester, is designated as BN-M-F.
2. nanometer AL2O3Processing procedure:By nanometer AL2O3(45g) is added to absolute ethyl alcohol(30ml)In, ultrasonic vibration Dispersion 30min, then by AL2O3It is 5 with KH550 mass ratioes:1 ratio adds KH550, and 400rpm is pressed in microwave reactor Speed stirring, 40 ~ 100 DEG C of 20 ~ 60min of reaction, high speed centrifugation removes unnecessary KH550, and through drying, milling obtains KH550 The AL of modification2O3-M。
By the modified AL of above-mentioned 10g2O3- M, 1molN, N- dihydroxy ethyl -3- amido methyl propionate monomers and 1g are to toluene sulphur Acid is placed in flask and puts into microwave generator, in N2The speed stirring 5h of 400rpm is pressed under protection in 130 DEG C.Vacuumize 30min obtains containing the nanometer AL being grafted to remove unreacted monomer2O3, the method being then centrifuged for is washed with methyl alcohol and washes dry Resulting polymers are vacuum dried 4h by net polymer in 80 DEG C, obtain the ester modified nanometer AL of hyperbranched polyamine2O3, it is designated as AL2O3-M-F。
By nanometer BN-M-F and nanometer AL2O3- M-F presses 1:Ball milling dispersion is equal in organic solvent after 5 mass ratio mixing It is even, it is then added in epoxy resin, addition is the 10% of epoxy resin quality, presses 400rpm's in microwave reactor Speed is stirred, and 100 ~ 120 DEG C continue 60min, then ultrasonic wave dispersion 30min, and epoxy resin used is the epoxy of bisphenol A-type -144 Resin, is its 20% aliphatic amine type curing agent by made epoxide resin encapsulation material and mass ratio(Ethylenediamine)After deployed Directly its thermal conductivity factor is tested in solidification to a part, and its reaction speed is tested in another part embedding in bullet-shaped thermistor. The results are shown in Table 1 and table 2.
Embodiment 2:
1. the processing procedure of nanometer BN:10g nanometers of BN is weighed, 400ml anhydrous dioxanes surpass in the flask of 2500ml Dispersion 30min is swung in acoustic shock, then by BN and hexamethylene diisocyanate(HDI)Mass ratio is 6:1 ratio adds six methylenes Group diisocyanate and 0.5mml catalyst dibutyltin cinnamic acid dibutyl alkene(DBTDL), the speed of 400rpm is pressed in microwave reactor Rate is stirred, and 40 ~ 120 DEG C of 20 ~ 60min of reaction, cooling room temperature filtering, high speed centrifugation removes unnecessary HDI, through drying, mills To the BN-M modified through HDI.
Weigh above-mentioned BN-M10g, hyper-branched polyester H20 38.5g(23.8ml)With 1000ml anhydrous dioxanes, together It is added in flask, is passed through argon gas protection, add the DBTDL of 0. 5ml, is stirred by the speed of 400rpm in microwave reactor Mix, 75 DEG C of reaction 12h, just resulting polymers are vacuum dried 4h in 80 DEG C after removing unnecessary H20 and washes clean, are surpassed The modified nanometer BN of branched polyester, is designated as BN-M-F.
2. nanometer AL2O3Processing procedure:By nanometer AL2O3(45g) is added to absolute ethyl alcohol(30ml)In, ultrasonic vibration Dispersion 30min, then by AL2O3It is 5 with KH550 mass ratioes:1 ratio adds KH550, and 400rpm is pressed in microwave reactor Speed stirring, 40 ~ 100 DEG C of 20 ~ 60min of reaction, high speed centrifugation removes unnecessary KH550, and through drying, milling obtains KH550 The AL of modification2O3-M。
By the modified AL of above-mentioned 10g2O3- M, 1molN, N- dihydroxy ethyl -3- amido methyl propionate monomers and 1g are to toluene sulphur Acid is placed in flask and puts into microwave generator, in N2The speed stirring 5h of 400rpm is pressed under protection in 130 DEG C.Vacuumize 30min obtains containing the nanometer AL being grafted to remove unreacted monomer2O3, the method being then centrifuged for is washed with methyl alcohol and washes dry Resulting polymers are vacuum dried 4h by net polymer in 80 DEG C, obtain the ester modified nanometer AL of hyperbranched polyamine2O3, it is designated as AL2O3-M-F。
By nanometer BN-M-F and nanometer AL2O3- M-F presses 2:Ball milling dispersion is equal in organic solvent after 5 mass ratio mixing It is even, it is then added in epoxy resin, addition is the 15% of epoxy resin quality, presses 400rpm's in microwave reactor Speed is stirred, and 100 ~ 120 DEG C continue 90min, then ultrasonic wave dispersion 30min, and epoxy resin used is the epoxy of bisphenol A-type -144 Resin, is its 20% aliphatic amine type curing agent by made epoxide resin encapsulation material and mass ratio(Ethylenediamine)After deployed Directly its thermal conductivity factor is tested in solidification to a part, and another part tests its reaction speed in the embedding in bullet-shaped thermistor Degree.The results are shown in Table 1 and table 2.
Embodiment 3:
1. the processing procedure of nanometer BN:10g nanometers of BN is weighed, 400ml anhydrous dioxanes surpass in the flask of 2500ml Dispersion 30min is swung in acoustic shock, then by BN and hexamethylene diisocyanate(HDI)Mass ratio is 6:1 ratio adds six methylenes Group diisocyanate and 0. 5mml catalyst dibutyltin cinnamic acid dibutyl alkene(DBTDL), the speed of 400rpm is pressed in microwave reactor Rate is stirred, and 40 ~ 120 DEG C of 20 ~ 60min of reaction, cooling room temperature filtering, high speed centrifugation removes unnecessary HDI, through drying, mills To the BN-M modified through HDI.
Weigh above-mentioned BN-M10g, hyper-branched polyester H20 38.5g(23.8ml)With 1000ml anhydrous dioxanes, together It is added in flask, is passed through argon gas protection, add the DBTDL of 0. 5ml, is stirred by the speed of 400rpm in microwave reactor Mix, 75 DEG C of reaction 12h, just resulting polymers are vacuum dried 4h in 80 DEG C after removing unnecessary H20 and washes clean, are surpassed The modified nanometer BN of branched polyester, is designated as BN-M-F.
2. nanometer AL2O3Processing procedure:By nanometer AL2O3(45g) is added to absolute ethyl alcohol(30ml)In, ultrasonic vibration Dispersion 30min, then by AL2O3It is 5 with KH550 mass ratioes:1 ratio adds KH550, and 400rpm is pressed in microwave reactor Speed stirring, 40 ~ 100 DEG C of 20 ~ 60min of reaction, high speed centrifugation removes unnecessary KH550, and through drying, milling obtains KH550 The AL of modification2O3-M。
By the modified AL of above-mentioned 10g2O3- APS, 1molN, N- dihydroxy ethyl -3- amido methyl propionate monomers and 1g are to toluene Sulfonic acid is placed in flask and puts into microwave generator, in N2The speed stirring 5h of 400rpm is pressed under protection in 130 DEG C.Vacuumize 30min obtains containing the nanometer AL being grafted to remove unreacted monomer2O3, the method being then centrifuged for is washed with methyl alcohol and washes dry Resulting polymers are vacuum dried 4h by net polymer in 80 DEG C, obtain the ester modified nanometer AL of hyperbranched polyamine2O3, it is designated as AL2O3-M-F。
By nanometer BN- M-F and nanometer AL2O3- M-F presses 4:Ball milling dispersion is equal in organic solvent after 5 mass ratio mixing It is even, it is then added in epoxy resin, addition is the 20% of epoxy resin quality, presses 400rpm's in microwave reactor Speed is stirred, and 100 ~ 120 DEG C continue 120min, then ultrasonic wave dispersion 30min, and epoxy resin used is the ring of bisphenol A-type -151 Oxygen tree fat, is its 20% aliphatic amine type curing agent by made epoxide resin encapsulation material and mass ratio(Ethylenediamine)It is deployed Rear portion directly solidifies tests its thermal conductivity factor, and its reaction speed is tested in another part embedding in bullet-shaped thermistor Degree.The results are shown in Table 1 and table 2.
Embodiment 4:
Nanometer BN and nanometer AL in this example2O31 is directly pressed without hyperbranched treatment:Organic after 5 mass ratio mixing Ball milling is uniformly dispersed in solvent, is then added in epoxy resin, and addition is the 10% of epoxy resin quality, anti-in microwave Answer in device and stirred by the speed of 400rpm, 100 ~ 120 DEG C continue 60min, then ultrasonic wave dispersion 30min, epoxy resin used It is the epoxy resin of bisphenol A-type -144, is its 20% aliphatic amine type curing agent by made epoxide resin encapsulation material and mass ratio (Ethylenediamine)Deployed rear portion directly solidifies tests its thermal conductivity factor, and another part is filled in bullet-shaped thermistor Envelope, tests its reaction speed.The results are shown in Table 1 and table 2.
Embodiment 5:
Epoxy resin in this example is the epoxy resin of bisphenol A-type -144, without nanometer BN and nanometer AL2O3, directly and Quality is its 20% aliphatic amine type curing agent(Ethylenediamine)Deployed rear portion directly solidifies tests its thermal conductivity factor, another Part embedding in bullet-shaped thermistor, tests its reaction speed.The results are shown in Table 1 and table 2.
The thermal conductivity factor of the example epoxy resin of table 1
The thermistor reaction speed that the different potting compounds of table 2 make

Claims (9)

1. be modified the preparation method of high thermal conductivity coefficient thermistor epoxide resin encapsulation material, it is characterised in that:Comprise the following steps:
1)The moditied processing of the first inorganic nano-filler:First inorganic nano-filler, isocyanates, catalyst are mixed in organic molten In agent, fully reaction, separation of solid and liquid, gained solid is fully dried, and grinding obtains the filler of isocyanate-modified;
2)The filler of isocyanate-modified, hyper-branched polyester, catalyst are placed in organic solvent, under protective atmosphere, fully Reaction, products therefrom is separated, and is washed, and is fully dried, and obtains modified filler 1;
3)The moditied processing of the second inorganic nano-filler:Second inorganic nano-filler, coupling agent are mixed in organic solvent, fully Reaction, isolates product, obtains the filler of coupling agent modification;
4)Filler, activated monomer, the catalyst mixing that coupling agent is modified, under protective atmosphere, are fully reacted, and separation is produced Thing, washing is dried, and obtains modified filler 2;
5)Modified filler 1 and modified filler 2 is dispersed in the epoxy;
Described activated monomer is N, N- dihydroxy ethyl -3- amido methyl propionates.
2. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 1, it is special Levy and be:Described the first inorganic nano-filler, the second inorganic nano-filler are independently selected from following inorganic nano-filler In at least one:BN、Al2O3、AlN、MgO、ZnO、SiO2、Si3N4, SiC, BeO, carbon dust, Graphene, graphite powder.
3. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 1 and 2, its It is characterised by:Described isocyanates is in MDI, HDI, NDI, PPDI, IPDI, XDI, TDI, PAPI, HTDI, HMDI, CHDI At least one.
4. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 3, it is special Levy and be:Described hyper-branched polyester be Boltorn H20, Boltorn H30, Boltorn H40, Boltorn U3000, At least one in Boltorn W3000, Boltorn H2004.
5. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 4, it is special Levy and be:Described coupling agent be silane coupler, titanate coupling agent, aluminate coupling agent, zirconium ester coupling agent in extremely Few one kind.
6. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 1, it is special Levy and be:Step 1)In, the first inorganic nano-filler, the mass ratio of isocyanates are(5-20):1.
7. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 6, it is special Levy and be:Step 2)In, the filler of isocyanate-modified, the amount ratio of hyper-branched polyester are:1g :(2-10)mL.
8. the preparation method of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material according to claim 7, it is special Levy and be:Step 3)In, the mass ratio of the second inorganic nano-filler and coupling agent is(1-20):1 ;Step 4)In, coupling agent is repaiied The filler of decorations, the amount ratio of activated monomer are(5-20)g :1mol.
9. application of the epoxide resin encapsulation material that prepared by the method for claim 8 in high thermal conductivity coefficient thermistor is prepared.
CN201510704833.0A 2015-10-27 2015-10-27 A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material Active CN105255111B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510704833.0A CN105255111B (en) 2015-10-27 2015-10-27 A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510704833.0A CN105255111B (en) 2015-10-27 2015-10-27 A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material

Publications (2)

Publication Number Publication Date
CN105255111A CN105255111A (en) 2016-01-20
CN105255111B true CN105255111B (en) 2017-06-30

Family

ID=55095079

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510704833.0A Active CN105255111B (en) 2015-10-27 2015-10-27 A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material

Country Status (1)

Country Link
CN (1) CN105255111B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108047456B (en) * 2017-09-01 2021-01-15 深圳市深大极光科技有限公司 Preparation method of BN nanosheet, photopolymer coating, thin film material and preparation method
CN111606693A (en) * 2020-06-01 2020-09-01 东阳市聚冉电子科技有限公司 Preparation method of high-temperature negative temperature coefficient thermistor material
CN112063086A (en) * 2020-09-23 2020-12-11 初殿德 Environment-friendly toy material and preparation method thereof
CN113372107B (en) * 2021-07-08 2023-01-31 铜陵四拓智能装备科技有限公司 Preparation process of low-thermal-expansion composite material
CN114999752A (en) * 2022-05-27 2022-09-02 广东新成科技实业有限公司 NTC patch thermistor based on semiconductor material and preparation method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100491490C (en) * 2006-11-09 2009-05-27 上海大学 Low-viscosity heat-conductive adhesive and process for preparing same
CN102876107B (en) * 2012-10-08 2014-09-17 中国船舶重工集团公司第七一二研究所 Heat-conduction insulating varnish composite material and preparation method thereof
CN104910845B (en) * 2015-06-12 2017-11-07 深圳先进技术研究院 Underfill and preparation method thereof

Also Published As

Publication number Publication date
CN105255111A (en) 2016-01-20

Similar Documents

Publication Publication Date Title
CN105255111B (en) A kind of preparation method and application of modified high thermal conductivity coefficient thermistor epoxide resin encapsulation material
CN107793992B (en) A kind of additional organosilicon casting glue and preparation method thereof
CN104098914B (en) Organosilicon heat-conducting interface material
JP2570002B2 (en) Flip chip sealing material and semiconductor device
US8664629B2 (en) Boron cage compound materials and composites for shielding and absorbing neutrons
CN107955412B (en) Preparation method and application of modified nano silicon dioxide
CN103665885B (en) A kind of High tear resistance silicon rubber and preparation method thereof
CN106281206A (en) A kind of electrostatic-resistant heat conducting organosilicon adhesive
CN103013124A (en) High-curing-speed, high-storage-stability and humidity/heat-resistant de-oximed room temperature vulcanized silicone rubber for new energy and preparation method thereof
CN103409103A (en) Environment-friendly high-temperature-resistant organic silicon pressure-sensitive adhesive and preparation method thereof
CN109554159A (en) A kind of LED silicone insulation crystal-bonding adhesive and preparation method thereof
CN107312495A (en) A kind of tack high-temperature silicon disulfide rubber band and preparation method thereof
CN105960426A (en) Resin composition, resin film, and semiconductor device and method for manufacturing same
CN101787256A (en) Addition type silicone adhesive composition and preparation method thereof
CN101817999B (en) Preparation method of twice-modified white carbon black
CN113861406A (en) Method for preparing silane modified polyether by using dichlorosilane
CN110845989B (en) Two-component organic silicon pouring sealant and application method thereof
CN106831845A (en) Boracic organo-silicon compound, Preparation Method And The Use
CN113185947A (en) Mixed crosslinking system two-component hollow sealant
CN108504315A (en) A kind of high temperature resistant casting glue and preparation method thereof
CN108192349A (en) A kind of dealcoholized type room temperature vulcanized silicone rubber and preparation method thereof
CN107325264A (en) Resin combination, resin film, the manufacture method of resin film, the manufacture method of semiconductor device and semiconductor device
CN105778100B (en) A kind of organic silicon rigidity-increasing stick and preparation method thereof and a kind of addition-type silicon rubber composition
CN106497476A (en) A kind of high heat conduction mica tape organic/inorganic composite adhesive and preparation method thereof
KR101284764B1 (en) Epoxy Compositions Having Enhanced Heat Conductivity

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CP01 Change in the name or title of a patent holder
CP01 Change in the name or title of a patent holder

Address after: No.4, Canghai 4th Road, Yonghe Economic Zone, Guangzhou Economic and Technological Development Zone, Guangzhou, Guangdong 511356

Patentee after: Guangzhou xinlaifu New Material Co.,Ltd.

Address before: No.4, Canghai 4th Road, Yonghe Economic Zone, Guangzhou Economic and Technological Development Zone, Guangzhou, Guangdong 511356

Patentee before: Guangzhou Newlife Magnet Electricity Co.,Ltd.