CN107523013A - A kind of resin composite materials and its production and use and heat conducting element and electrical equipment - Google Patents
A kind of resin composite materials and its production and use and heat conducting element and electrical equipment Download PDFInfo
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- CN107523013A CN107523013A CN201610473798.0A CN201610473798A CN107523013A CN 107523013 A CN107523013 A CN 107523013A CN 201610473798 A CN201610473798 A CN 201610473798A CN 107523013 A CN107523013 A CN 107523013A
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- boron nitride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V29/00—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems
- F21V29/85—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems characterised by the material
- F21V29/87—Organic material, e.g. filled polymer composites; Thermo-conductive additives or coatings therefor
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Abstract
Heat conducting element and electrical equipment the invention discloses a kind of resin composite materials and its production and use and comprising the resin composite materials, the hydroxylated boron nitride that the resin composite materials include the epoxy resin of solidification and are distributed in the epoxy resin of the solidification, hydroxy radical content in the hydroxylated boron nitride is 0.04 0.15mmol/g, on the basis of the gross weight of the resin composite materials, the content of the hydroxylated boron nitride is 5 40 weight %.The heat conducting element prepared using the resin composite materials has good fire resistance, is continuously worked available for great power LED, improves LED job stability.
Description
Technical field
The present invention relates to resin material processed and applied field.
Background technology
LED has the characteristics that energy-saving and environmental protection, long lifespan, small volume as forth generation lighting source,
But substituting traditional light source to also face many technological difficulties completely, wherein heat dissipation problem is limitation LED
One key factor of light fixture especially high-powered LED lamp development.
Most of LED cooling lamp holders material on the market is plastics, aluminium or copper at present.Metal
Material thermal conductivity factor is big, and thermal resistance is small, and rate of heat transfer is fast, and heat dispersion is more preferable, but its density is big, cost
High and processing relative difficulty, further, since metal material is conductive, is prepared using metal material
The potential safety hazard of electric leakage also be present in LED cooling lamp holders.Heat-conducting plastic density is small, light weight, substantially reduces
Cost of transportation, its characteristic being electrically insulated are even more the security for improving and using, in process can be with
Using injection molding, improve design freedom and shorten the duration simultaneously, but its thermal conductivity is relatively low, and hinder
Combustion property is very poor, limits its application in high-power LED radiator.
The content of the invention
It is an object of the invention to provide a kind of resin composite materials and its production and use and comprising
The heat conducting element and electrical equipment of the resin composite materials, the heat conducting element prepared using the resin composite materials are had
There are good heat conduction and fire resistance, continuously worked available for great power LED, improve LED work
Stability.
To achieve these goals, first aspect present invention：A kind of resin composite materials, the tree are provided
The hydroxylating that resin composite material includes the epoxy resin of solidification and is distributed in the epoxy resin of the solidification
Boron nitride, the hydroxy radical content in the hydroxylated boron nitride is 0.04-0.15mmol/g, with the tree
On the basis of the gross weight of resin composite material, the content of the hydroxylated boron nitride is 5-40 weight %.
Preferably, the hydroxy radical content in the hydroxylated boron nitride is 0.08-0.10mmol/g.
Preferably, on the basis of the gross weight of the resin composite materials, the hydroxylated boron nitride
Content is 5-20 weight %.
Preferably, the epoxy resin of the solidification be by epoxide equivalent for 172-195 grams/equivalent solidification before
Epoxy resin cure obtain.
Preferably, the epoxy resin of the solidification is included in bisphenol A epoxide resin and phenol aldehyde type epoxy resin
At least one.
Second aspect of the present invention, there is provided a kind of method for preparing resin composite materials, this method include as follows
Step：A, boron nitride raw is contacted with hydroxylating agent, the material after being contacted, and separates institute
The solid in the material after contact is stated to obtain hydroxylated boron nitride；The condition of contact causes the hydroxyl
Hydroxy radical content in the boron nitride of change is 0.04-0.15mmol/g；The hydroxylating agent include hydrogen peroxide,
At least one of TBHP and cyclohexyl hydroperoxide；B, by the epoxy resin before solidification,
Curing agent mixes with the hydroxylated boron nitride obtained in step a and carries out curing process, is set
Resin composite material.
Preferably, the condition contacted described in step a is：Temperature is 90 DEG C -100 DEG C, time 10-24
Hour.
Preferably, in step b, on the basis of the gross weight of the resin composite materials, the hydroxylating
The content of boron nitride be 5-40 weight %.
Preferably, the epoxide equivalent of the epoxy resin in step b is 172-195 grams/equivalent.
Preferably, the epoxy resin in step b includes bisphenol A epoxide resin and phenolic epoxy tree
At least one of fat.
Preferably, the curing agent in step b includes diethylenetriamine, triethylene tetramine and maleic
At least one of dicarboxylic anhydride.
Preferably, this method is additionally included in step b, the hydroxylated nitridation that will first be obtained in step a
Boron is ultrasonically treated, and is then mixed again with the epoxy resin before the solidification.
Preferably, the curing process in step b include the first curing process, the second curing process and
3rd curing process, the temperature of first curing process is 20-40 DEG C, and the time is 5-12 hours；Institute
The temperature for stating the second curing process is 60-80 DEG C, and the time is 5-10 hours；3rd curing process
Temperature is 120-150 DEG C, and the time is 8-12 hours
Third aspect present invention, there is provided the resin composite materials of first aspect present invention are preparing heat conducting element
In purposes.
Fourth aspect present invention, there is provided a kind of heat conducting element, the heat conducting element contain first aspect present invention
Resin composite materials.
Fifth aspect present invention, there is provided a kind of electrical equipment, the electrical equipment contain the heat conduction member of fourth aspect present invention
Part.
Preferably, the electrical equipment is LED bulb.
Pass through above-mentioned technical proposal, resin composite materials provided by the invention have higher oxygen index (OI) and heat
Conductance, the heat conducting element fire resistance and good heat conductivity prepared using the resin composite materials, can be used for
In great power LED electrical equipment, LED electrical work stability is improved, in addition, also having light weight, is made
With it is safe the features such as.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It should be appreciated that this place is retouched
The embodiment stated is merely to illustrate and explain the present invention, and is not intended to limit the invention.
First aspect present invention, there is provided a kind of resin composite materials, the resin composite materials include solidification
Epoxy resin and the hydroxylated boron nitride that is distributed in the epoxy resin of the solidification, the hydroxylating
Boron nitride in hydroxy radical content can be 0.04-0.15mmol/g, with the gross weight of the resin composite materials
On the basis of amount, the content of the hydroxylated boron nitride can be 5-40 weight %.Tree provided by the invention
Resin composite material can reduce the contact area of epoxy resin and air using boron nitride, so as to improve resin
The oxygen index (OI) of composite, its oxygen index (OI) can reach in the case of the boron nitride added with lower content
More than 22, there is good fire resistance.
According to the first aspect of the invention, in order to obtain more preferable flame retardant effect, at the same keep it is good can
Processability, the hydroxy radical content in the hydroxylated boron nitride is preferably 0.08-0.10mmol/g, with described
On the basis of the gross weight of resin composite materials, the content of the hydroxylated boron nitride is preferably 5-20 weights
Measure %.
According to the first aspect of the invention, in order to reach higher thermal conductivity, the epoxy resin of the solidification
It is to be obtained by epoxide equivalent for the epoxy resin cure before the solidification of 172-195 grams/equivalent.The solidification
Epoxy resin can include at least one of bisphenol A epoxide resin and phenol aldehyde type epoxy resin.
Second aspect of the present invention, there is provided a kind of method for preparing resin composite materials, this method include as follows
Step：A, boron nitride raw is contacted with hydroxylating agent, the material after being contacted, and separates institute
The solid in the material after contact is stated to obtain hydroxylated boron nitride；The condition of contact causes the hydroxyl
Hydroxy radical content in the boron nitride of change is 0.04-0.15mmol/g；The hydroxylating agent include hydrogen peroxide,
At least one of TBHP and cyclohexyl hydroperoxide；B, by the epoxy resin before solidification,
Curing agent mixes with the hydroxylated boron nitride obtained in step a and carries out curing process, is set
Resin composite material.The sclay texture of boron nitride can reduce the contact area of epoxy resin and air, from
And the oxygen index (OI) of resin composite materials is improved, improve fire resistance, boron nitride raw is subjected to hydroxylating more
Be advantageous to it to be mixed with epoxy resin.
According to the second aspect of the invention, the ingredient proportion of boron nitride raw and hydroxylating agent does not have in step a
There is special limitation, as long as hydroxylating agent is flooded into boron nitride raw contacted with reaching described in step a
Purpose.In order to improve the contacting efficiency of boron nitride raw and hydrogen peroxide, heating can be used, stirred
The method for the conventional increase reaction rate such as mixing.Material after contact can use conventional solid-liquid separating method
Separated, such as filter, evaporate, drying.The temperature of the contact can be 90-100 DEG C, contact
Time can be 12-24 hours.
According to the second aspect of the invention, in order to obtain more preferable flame retardant effect, at the same keep it is good can
Processability, in step b, on the basis of the gross weight of the resin composite materials, the hydroxylated nitrogen
The content for changing boron can be 5-40 weight %, preferably 5-20 weight %.In order that before the solidification
Epoxy resin is well mixed with hydroxylated boron nitride, can use the side of conventional raising mixed effect
Method, such as stir.In addition, in order to improve solidification before epoxy resin mixed with hydroxylated boron nitride after
Mixture mobility, solvent can also be added into the mixture, the solvent can be selected from second
Alcohol and/or acetone.
According to the second aspect of the invention, in order to reach higher thermal conductivity, the epoxy in step b
The epoxide equivalent of resin can be 172-195 grams/equivalent, preferably 180-190 grams/equivalent.The epoxy
Resin includes at least one of bisphenol A epoxide resin and phenol aldehyde type epoxy resin.
According to the second aspect of the invention, the curing agent in step b can be the conventional choosing of this area
Select, such as at least one of diethylenetriamine, triethylene tetramine and maleic anhydride can be included.With
Epoxy resin before the solidification and on the basis of the gross weight of curing agent, the content of the curing agent can be
11-30 weight %.
According to the second aspect of the invention, in order that hydroxylated boron nitride be easier to before the solidification
Epoxy resin is well mixed, and this method is additionally included in step b, the hydroxylating that will first be obtained in step a
Boron nitride be ultrasonically treated, then mixed again with the epoxy resin before solidification.After supersound process,
The hydroxylated boron nitride has sclay texture, can more preferable air-isolation, further increase
The fire resistance of resin composite materials.
According to the second aspect of the invention, mixed to remove the epoxy resin before the solidification with boron nitride
Bubble, solvent in the mixture obtained afterwards, first the mixture can be fallen before curing process is carried out
Enter and the first vacuumize process is carried out in mould, the vacuum of first vacuumize process can be 10-30
Pa, time can be 1-3 hours.The mixture is at least partially dried after first vacuumize process, in order to
Make final resin composite materials product finer and close, can also be to the mixture after the first vacuumize process
Carry out the second vacuumize process, the vacuum of second vacuumize process can be 10-30Pa, the time
Can be 1-5 hours, the basic forming of the mixture after the second vacuumize process.
According to the second aspect of the invention, in order to avoid producing bubble, step b during curing process
In the curing process can include the first curing process, the second curing process and the 3rd curing process,
The temperature of first curing process can be 20-40 DEG C, and the time can be 5-12 hours；Described second
The temperature of curing process can be 60-80 DEG C, and the time can be 5-10 hours；3rd curing process
Temperature can be 120-150 DEG C, the time can be 8-12 hours.
The method of second aspect of the present invention is thrown after being additionally included in the processing that is heating and curing in step b
The step of light, polishing.
Third aspect present invention, there is provided the resin composite materials of first method of the present invention are preparing heat conducting element
In purposes.
Fourth aspect present invention, there is provided a kind of heat conducting element, the heat conducting element contain first method of the present invention
Resin composite materials.The heat conducting element is had compared with the radiator prepared using conventional thermal conductive plastics
More preferable flame retardant effect and radiating effect, and light weight, safety in utilization are good.
Fifth aspect present invention, there is provided a kind of electrical equipment, the electrical equipment contain the heat conduction member of fourth aspect present invention
Part.Further, the electrical equipment can be LED bulb.As a result of fourth aspect present invention
Heat conducting element, reduce LED bulb and the probability for leading to not work is burnt out due to weak heat-dissipating, in pole
Will not ignition in the case of end so that the job stability of LED bulb is more preferable, and security is higher.
The present invention is further illustrated below by embodiment, but the present invention is not therefore and by any limit
System.
Boron nitride P100 employed in embodiment and comparative example is purchased from the limited public affairs of brilliant hundred million ceramics in Zibo
Department, bisphenol A epoxide resin (epoxide equivalent is 172-176 grams/equivalent) and phenol aldehyde type epoxy resin (ring
Oxygen equivalent is 185-195 grams/equivalent) it is purchased from Shenzhen Suncor Inc. (CA) 500-4th Avenue S.W., Calgary, Alberta, T2P2V5. Canada.The power of LED bulb be 3W and
9W。
Hydroxy radical content in hydroxylated boron nitride is using Thermo Fisher Scienctific companies
ESCALAB 250 model x-ray photoelectron spectroscopies are measured, and test condition is vacuum 1.2 × 10-9
Mbar, use aluminium target Al K α X ray (1486.6eV).The oxygen index (OI) of resin composite materials uses Britain
The FTT08-1 type oxygen index measurers of FTT companies are measured, and it is propane to light gas, according to GB/T
2406.2-2009 standard method is measured.
Embodiment 1
400g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, it is double
Oxygen water submerged boron nitride raw, water heating kettle is put into baking oven, cooled after 100 DEG C of holding 24h, mistake
Filter, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.15mmol/g.By 400g hydroxyls
After the boron nitride ultrasound 1h of change, bisphenol A epoxide resin and 66g curing agent diethyls before solidifying with 534g
Alkene triamine, which is placed in beaker, to be mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h, vacuum
Spend for 30Pa, then heat to 40 DEG C and kept for 12 hours, then be warming up to 80 DEG C of holding 5h, finally rise
Then temperature cools to 120 DEG C of holding 8h, obtains resin composite materials.The oxygen of gained resin composite materials
Index is 25.6.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 3W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 33.9 DEG C,
And with after lighter calcination 5 seconds without burning and metaboly.It is commercially available under identical condition of work
Plastic LED radiator temperature is 27.7 DEG C, i.e. the LED bulb radiator of the present embodiment has more preferable
Radiating effect.
Embodiment 2
200g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, it is double
Oxygen water submerged boron nitride raw, water heating kettle is put into baking oven, cooled after 100 DEG C of holding 24h, mistake
Filter, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.10mmol/g.By 200g hydroxyls
After the boron nitride ultrasound 1h of change, bisphenol A epoxide resin and 88g curing agent two before solidifying with 712g
Ethene triamine, which is placed in beaker, to be mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h, very
Reciprocal of duty cycle is 30Pa, then heats to 30 DEG C and is kept for 10 hours, then is warming up to 70 DEG C of holding 6h, finally
140 DEG C of holding 10h are warming up to, then cools, obtains resin composite materials.Gained resin composite materials
Oxygen index (OI) be 27.6.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 3W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 36.8 DEG C,
With after lighter calcination 5 seconds without burning and metaboly.
Embodiment 3
100g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, it is double
Oxygen water submerged boron nitride raw, water heating kettle is put into baking oven, cooled after 100 DEG C of holding 24h, mistake
Filter, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.08mmol/g.By 100g hydroxyls
After the boron nitride ultrasound 1h of change, bisphenol A epoxide resin and the second of 99g curing agent three before solidifying with 801g
Alkene tetramine, which is placed in beaker, to be mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h, vacuum
Spend for 30Pa, then heat to 20 DEG C and kept for 8 hours, then be warming up to 60 DEG C of holding 10h, finally rise
Then temperature cools to 150 DEG C of holding 12h, obtains resin composite materials.Gained resin composite materials
Oxygen index (OI) is 26.8.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 9W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 38.4 DEG C,
With after lighter calcination 5 seconds without burning and metaboly.
Embodiment 4
100g boron nitride raws P100 is placed in water heating kettle, adds TBHP, the tert-butyl group
Hydrogen peroxide floods boron nitride raw, and water heating kettle is put into baking oven, cooled after 90 DEG C of holding 12h,
Filtering, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.04mmol/g.By 100g hydroxyls
After the boron nitride ultrasound 1h of base, bisphenol A epoxide resin and 380g curing agent before solidifying with 1520g
Triethylene tetramine is placed in beaker and mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h,
Vacuum is 30Pa, then heats to 40 DEG C and is kept for 12 hours, then is warming up to 80 DEG C of holding 5h, most
After be warming up to 120 DEG C holding 8h, then cool, obtain resin composite materials.Gained resin composite materials
Oxygen index (OI) be 26.0.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 3W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 34.6 DEG C,
With after lighter calcination 5 seconds without burning and metaboly.
Embodiment 5
400g boron nitride raws P100 is placed in water heating kettle, adds cyclohexyl hydroperoxide, cyclohexyl
Hydrogen peroxide floods boron nitride raw, and water heating kettle is put into baking oven, cooled after 90 DEG C of holding 24h,
Filtering, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.09mmol/g.By 400g hydroxyls
After the boron nitride ultrasound 1h of base, phenol aldehyde type epoxy resin and 180g curing agent before solidifying with 420g
Maleic anhydride is placed in beaker and mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h,
Vacuum is 30Pa, then heats to 40 DEG C and is kept for 12 hours, then is warming up to 80 DEG C of holding 5h, most
After be warming up to 150 DEG C holding 12h, then cool, obtain resin composite materials, then cool, obtain
Resin composite materials.The oxygen index (OI) of gained resin composite materials is 26.5.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 9W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 39.8 DEG C,
With after lighter calcination 5 seconds without burning and metaboly.
Embodiment 6
200g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, it is double
Oxygen water submerged boron nitride raw, water heating kettle is put into baking oven, cooled after 100 DEG C of holding 24h, mistake
Filter, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.08mmol/g.By 200g hydroxyls
After the boron nitride ultrasound 1h of change, the phenol aldehyde type epoxy resin and 88g curing agent before solidifying with 712g are along fourth
Enedioic acid acid anhydride, which is placed in beaker, to be mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h, very
Reciprocal of duty cycle is 10Pa, then heats to 40 DEG C and is kept for 12 hours, then is warming up to 80 DEG C of holding 5h, finally
150 DEG C of holding 12h are warming up to, then cools, obtains resin composite materials.Gained resin composite materials
Oxygen index (OI) is 26.1.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 9W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 40.1 DEG C,
With after lighter calcination 5 seconds without burning and metaboly.
Embodiment 7
300g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, it is double
Oxygen water submerged boron nitride raw, water heating kettle is put into baking oven, cooled after 100 DEG C of holding 12h, mistake
Filter, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.11mmol/g.By 300g hydroxyls
After the boron nitride ultrasound 1h of change, bisphenol A type epoxy resin and 77g curing agent two before solidifying with 623g
Ethene triamine, which is placed in beaker, to be mixed, and normal temperature in mould is poured into after stirring 0.5h and vacuumizes standing 1h, very
Reciprocal of duty cycle is 20Pa, then heats to 40 DEG C and is kept for 12 hours, then is warming up to 80 DEG C of holding 5h, finally
120 DEG C of holding 8h are warming up to, then cools, obtains resin composite materials.Gained resin composite materials
Oxygen index (OI) is 26.0.
After polishing by the resin composite materials of gained and polish radiating groove, heat conducting element is made, by this
Heat conducting element is used for LED bulb radiator, and the power of LED bulb used is 3W, LED bulb
After work 1 hour, the temperature of LED bulb radiator made of the heat conducting element is used as 35.7 DEG C,
With after lighter calcination 5 seconds without burning and metaboly.
Comparative example 1
Bisphenol A epoxide resin before 534g is solidified keeps entering for 8 hours with 66g curing agent at 120 DEG C
Row solidification, then cools, the bisphenol A epoxide resin after being solidified, and its oxygen index (OI) is 20.5.By its
For LED bulb radiator, the power of LED bulb used is 3W, and LED bulb work 1 is small
Shi Hou, the temperature of the radiator is 27.7 DEG C, and with lighter calcination, 5 seconds start to deform.
Comparative example 2
Bisphenol A epoxide resin and 66g curing agent before 400g boron nitride raws are solidified with 534g are placed in
Mixed in beaker, pour into standing 1h in mould after stirring 1h, 120 DEG C keep being solidified for 8 hours, so
After cool, obtain resin composite materials, its oxygen index (OI) be 21.6.LED bulb radiator is used it for,
The power of LED bulb used is 3W, after LED bulb works 1 hour, the temperature of the radiator
For 28.1 DEG C, with lighter calcination, 5 seconds start to deform.
Comparative example 3
400g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, will
Water heating kettle is put into baking oven, cools after 100 DEG C of holding 24h, filters, dries, obtain hydroxylated nitridation
Boron, its hydroxy radical content are 0.02mmol/g.Before the hydroxylated boron nitride of 400g and 534g solidifications
Bisphenol A epoxide resin and 66g curing agent are placed in beaker and mixed, and 120 DEG C keep being solidified for 8 hours,
Then cool, obtain resin composite materials, its oxygen index (OI) is 22.1.Use it for LED bulb radiating
Device, the power of LED bulb used is 3W, after LED bulb works 1 hour, the radiator
Temperature is 28.4 DEG C, and with lighter calcination, 5 seconds start to deform.
Comparative example 4
400g boron nitride raws P100 is placed in water heating kettle, adds 30 weight % hydrogen peroxide, it is double
Oxygen water submerged boron nitride raw, water heating kettle is put into baking oven, cooled after 100 DEG C of holding 24h, mistake
Filter, drying, obtain hydroxylated boron nitride, its hydroxy radical content is 0.15mmol/g.By 400g hydroxyls
The boron nitride of change and the phenol aldehyde type epoxy resin (epoxide equivalent is 200 grams/equivalent) before 534g solidifications and
66g curing agent, which is placed in beaker, to be mixed, and 120 DEG C keep being solidified for 8 hours, then cool, are set
Oil/fat composition composite, its oxygen index (OI) are 22.5.LED bulb radiator is used it for, it is used
The power of LED bulb is 3W, and after LED bulb works 1 hour, the temperature of the radiator is 28.5 DEG C,
With lighter calcination, 5 seconds start to deform.
The method using the present invention is can be seen that specific from embodiment 1-7 and comparative example 1-4 result
Hydroxylated boron nitride and the epoxy resin with specific epoxide number are mixed with obtained tree under ratio
Its oxygen index (OI) of resin composite material can reach more than 25.6, use it for high-power LED bulb radiator
Good fire resistance is shown, the temperature of the radiator is bought than market under identical condition of work
Plastic tank radiators temperature is high more than 6.2 DEG C, with using without boron nitride, the non-hydroxylating of boron nitride, hydroxyl
Radiator made of the hydroxy radical content deficiency and the unsuitable resin of epoxide equivalent of the boron nitride of change is compared
Temperature improve up to more than 12.4 DEG C, represent more preferable radiating effect, with after lighter calcination without change
Shape and combustion phenomena, so as to extend the service life of LED bulb and strengthen its security.
Claims (17)
1. a kind of resin composite materials, it is characterised in that the resin composite materials include the ring of solidification
Oxygen tree fat and the hydroxylated boron nitride being distributed in the epoxy resin of the solidification, the hydroxylated nitrogen
The hydroxy radical content changed in boron is 0.04-0.15mmol/g, using the gross weight of the resin composite materials as base
Standard, the content of the hydroxylated boron nitride is 5-40 weight %.
2. resin composite materials according to claim 1, wherein, the hydroxylated boron nitride
In hydroxy radical content be 0.08-0.10mmol/g.
3. resin composite materials according to claim 1, wherein, with the resin composite materials
Gross weight on the basis of, the content of the hydroxylated boron nitride is 5-20 weight %.
4. resin composite materials according to claim 1, wherein, the epoxy resin of the solidification
It is to be obtained by epoxide equivalent for the epoxy resin cure before the solidification of 172-195 grams/equivalent.
5. resin composite materials according to claim 4, wherein, the epoxy resin of the solidification
Including at least one of bisphenol A epoxide resin and phenol aldehyde type epoxy resin.
A kind of 6. method for preparing resin composite materials, it is characterised in that this method comprises the following steps：
A, boron nitride raw is contacted with hydroxylating agent, the material after being contacted, and described in separation
The solid in material after contact is to obtain hydroxylated boron nitride；The condition of contact causes the hydroxylating
Boron nitride in hydroxy radical content be 0.04-0.15mmol/g；The hydroxylating agent includes hydrogen peroxide, uncle
At least one of butylhydroperoxide and cyclohexyl hydroperoxide；
B, the hydroxylated nitridation that will be obtained in the epoxy resin before solidification, curing agent and step a
Boron mixes and carries out curing process, obtains resin composite materials.
7. according to the method for claim 6, wherein, the condition contacted described in step a is：
Temperature is 90 DEG C -100 DEG C, and the time is 10-24 hours.
8. the method according to claim 11, wherein, in step b, with the resin compounded material
On the basis of the gross weight of material, the content of the hydroxylated boron nitride is 5-40 weight %.
9. the method according to claim 11, wherein, the ring of the epoxy resin in step b
Oxygen equivalent is 172-195 grams/equivalent.
10. according to the method for claim 6, wherein, the epoxy resin in step b includes
At least one of bisphenol A epoxide resin and phenol aldehyde type epoxy resin.
11. according to the method for claim 6, wherein, the curing agent in step b includes two
At least one of ethene triamine, triethylene tetramine and maleic anhydride.
12. according to the method for claim 6, this method is additionally included in step b, first by step
The hydroxylated boron nitride obtained in a is ultrasonically treated, then again with the epoxy resin before the solidification
Mixing.
13. according to the method for claim 6, wherein, the curing process in step b includes
First curing process, the second curing process and the 3rd curing process, the temperature of first curing process are
20-40 DEG C, the time is 5-12 hours；The temperature of second curing process is 60-80 DEG C, and the time is
5-10 hours；The temperature of 3rd curing process is 120-150 DEG C, and the time is 8-12 hours.
14. purposes of the resin composite materials described in claim 1-5 in heat conducting element is prepared.
15. a kind of heat conducting element, it is characterised in that the heat conducting element contains described in claim 1-5
Resin composite materials.
16. a kind of electrical equipment, it is characterised in that the electrical equipment contains the heat conducting element described in claim 15.
17. electrical equipment according to claim 16, wherein, the electrical equipment is LED bulb.
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| CN201610473798.0A CN107523013B (en) | 2016-06-22 | 2016-06-22 | Resin composite material, preparation method and application thereof, heat conducting element and electric appliance |
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| CN201610473798.0A CN107523013B (en) | 2016-06-22 | 2016-06-22 | Resin composite material, preparation method and application thereof, heat conducting element and electric appliance |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194939A (en) * | 2019-06-26 | 2019-09-03 | 苏州太湖电工新材料股份有限公司 | A kind of the two-component epoxy pouring sealant and its application method of high heat conductive insulating |
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| US20050072334A1 (en) * | 2003-10-07 | 2005-04-07 | Saint-Gobain Performance Plastics, Inc. | Thermal interface material |
| CN103480329A (en) * | 2013-09-05 | 2014-01-01 | 深圳先进技术研究院 | Hexagonal boron nitride/graphene oxide composite adsorption material and preparation method thereof |
| US8685534B2 (en) * | 2004-06-15 | 2014-04-01 | Siemens Energy, Inc. | High thermal conductivity materials aligned within resins |
| CN105453707A (en) * | 2013-08-14 | 2016-03-30 | 电化株式会社 | Boron nitride/resin composite circuit board, and circuit board including boron nitride/resin composite integrated with heat radiation plate |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050072334A1 (en) * | 2003-10-07 | 2005-04-07 | Saint-Gobain Performance Plastics, Inc. | Thermal interface material |
| US8685534B2 (en) * | 2004-06-15 | 2014-04-01 | Siemens Energy, Inc. | High thermal conductivity materials aligned within resins |
| CN105453707A (en) * | 2013-08-14 | 2016-03-30 | 电化株式会社 | Boron nitride/resin composite circuit board, and circuit board including boron nitride/resin composite integrated with heat radiation plate |
| CN103480329A (en) * | 2013-09-05 | 2014-01-01 | 深圳先进技术研究院 | Hexagonal boron nitride/graphene oxide composite adsorption material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110194939A (en) * | 2019-06-26 | 2019-09-03 | 苏州太湖电工新材料股份有限公司 | A kind of the two-component epoxy pouring sealant and its application method of high heat conductive insulating |
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