CN116589864A - Preparation method of heat-conductive resin composition capable of maintaining high heat conductivity - Google Patents
Preparation method of heat-conductive resin composition capable of maintaining high heat conductivity Download PDFInfo
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- CN116589864A CN116589864A CN202310578565.7A CN202310578565A CN116589864A CN 116589864 A CN116589864 A CN 116589864A CN 202310578565 A CN202310578565 A CN 202310578565A CN 116589864 A CN116589864 A CN 116589864A
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- 239000011342 resin composition Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000000843 powder Substances 0.000 claims abstract description 54
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052582 BN Inorganic materials 0.000 claims abstract description 46
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012188 paraffin wax Substances 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 23
- 239000010439 graphite Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims description 70
- 239000000203 mixture Substances 0.000 claims description 31
- 238000000227 grinding Methods 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- -1 polyethylene terephthalate Polymers 0.000 claims description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 10
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- XRBXGZZMKCBTFP-UHFFFAOYSA-N 4-(2,2-dihydroxyethoxycarbonyl)benzoic acid Chemical compound OC(O)COC(=O)C1=CC=C(C(O)=O)C=C1 XRBXGZZMKCBTFP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 238000005886 esterification reaction Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 230000009477 glass transition Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 235000011837 pasties Nutrition 0.000 claims description 5
- 238000006068 polycondensation reaction Methods 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003063 flame retardant Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/092—Polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
-
- 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
Abstract
The invention discloses a preparation method of a heat-conducting resin composition capable of maintaining high heat conductivity, and particularly relates to the technical field of preparation of heat-conducting resins, comprising the following components in parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin. The prepared heat-conducting resin composition has good heat-conducting property, wherein the added aluminum oxide powder, boron nitride powder and graphite powder can effectively maintain high heat-conducting property, the added chlorinated paraffin has good flame retardant property, the flame retardant property and the adhesive property of the prepared heat-conducting resin composition can be improved, and the whole preparation process flow is simple, the preparation cost is low, the equipment requirement is low, and the operability is strong.
Description
Technical Field
The present invention relates to the technical field of preparation of heat conductive resins, and more particularly, to a preparation method of a heat conductive resin composition capable of maintaining high heat conductivity.
Background
A semiconductor such as a Computer (CPU), a transistor, a Light Emitting Diode (LED) and the like generates heat during use, and the performance of an electronic component is sometimes degraded by the heat, and therefore, a radiator is mounted on the generated heat electronic component, but since most of the radiator is made of metal, the electronic component and the radiator portion are not well adhered, and therefore, a method of improving adhesion by inserting a thermally conductive resin composition formed into a sheet shape is adopted, but in recent years, the performance of an electronic device is remarkably improved, and the heat generation amount is also increased, and therefore, the research on the high thermal conductivity of the thermally conductive resin composition polymer composition is very active.
In recent years, as the performance of computers and electronic devices has increased, importance has increased in heat dissipation measures, and hexagonal boron nitride has been attracting attention as a filler having a high thermal conductivity resin composition, insulation properties, and the like, and chinese patent publication No. CN107922743B discloses a thermal conductivity resin composition, whereby a heat dissipation member excellent in thermal conductivity and dielectric breakdown properties can be provided. The mixing ratio of spherical boron nitride micro powder with the average grain diameter of 0.05-1.0 mu m, the average circularity of more than 0.80 and the purity of boron nitride of more than 96 mass percent and coarse boron nitride powder with the average grain diameter of 20-85 mu m and the graphitization index of 1.5-4.0 is 5: 95-40: 60, and the total content of the spherical boron nitride fine powder and the boron nitride coarse powder in the resin composition is 40 to 85% by volume.
In summary, although the thermal conductive resin compositions prepared in the prior art have good thermal conductive properties, the thermal conductive resin compositions prepared integrally have unsatisfactory flame retardant properties and adhesion properties, and the overall preparation process flow is complex and the preparation cost is high.
Disclosure of Invention
The technical scheme of the invention aims at solving the technical problem that the prior art is too single, provides a solution which is obviously different from the prior art, and aims to overcome the defects of the prior art, and provides a preparation method of a heat-conductive resin composition capable of maintaining high heat conductivity so as to solve the technical problem in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions: a thermally conductive resin composition capable of maintaining high thermal conductivity, characterized by comprising the following components in parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin.
As a further improvement of the technical scheme of the invention, the invention comprises the following components in parts by weight: 25-35 parts of terephthalic acid, 3-5 parts of aluminum oxide, 8-12 parts of boron nitride, 3-5 parts of graphite, 2-4 parts of deionized water, 4-6 parts of copper powder, 6-9 parts of ethylene glycol and 4-6 parts of chlorinated paraffin.
As a further improvement of the technical scheme of the invention, the invention comprises the following components in parts by weight: 30 parts of terephthalic acid, 4 parts of aluminum oxide, 10 parts of boron nitride, 4 parts of graphite, 3 parts of deionized water, 5 parts of copper powder, 8 parts of ethylene glycol and 5 parts of chlorinated paraffin.
A method for producing a thermally conductive resin composition capable of maintaining high thermal conductivity, comprising the steps of:
step one, preparing raw materials, wherein the raw materials comprise the following parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin;
grinding the solid powder, and sequentially placing aluminum oxide, boron nitride and graphite into a grinder to obtain aluminum oxide powder, boron nitride powder and graphite powder;
step three, preparing polyethylene glycol terephthalate, namely firstly synthesizing dihydroxyethyl terephthalate by esterification reaction of terephthalic acid and ethylene glycol, and then performing polycondensation reaction to prepare the polyethylene glycol terephthalate;
step four, preparing slurry, namely synchronously and slowly adding the alumina powder, the boron nitride powder and the graphite powder prepared in the step two into a stirring kettle, continuously stirring deionized water in the stirring kettle for 40-60min after the three powders are uniformly mixed until the mixture in the stirring kettle is pasty, and obtaining the slurry;
step five, preparing a mixture, namely adding the polyethylene terephthalate prepared in the step three and the slurry prepared in the step four into the same stirring kettle, heating the stirring kettle, stirring for 5min, adding chlorinated paraffin into the stirring kettle, and continuously stirring for 30-60min to obtain a mixture;
and step six, molding, namely taking out the mixture prepared in the step five, placing the mixture into a glass container, and naturally cooling the mixture to obtain the heat-conducting resin composition.
As a further improvement of the technical scheme of the invention, in the second step, the grinding speed of the grinder is controlled to be 500-800r/min, the grinding time is controlled to be 30-60min, and the fineness of the solid powder obtained after grinding is controlled to be 200-300 meshes.
As a further improvement of the technical scheme of the invention, the polyethylene terephthalate prepared in the third step has the average molecular weight (2-3). Times.104, the glass transition temperature of 80 ℃, the Martin heat resistance of 80 ℃, the heat distortion temperature of 98 ℃ (1.82 MPa) and the decomposition temperature of 353 ℃.
As a further improvement of the technical scheme of the invention, in the fourth step, the mixing time of the alumina powder, the boron nitride powder and the graphite powder in the stirring kettle is not less than 30min, the stirring speed is controlled to be 1200-1500 r/min, and the internal temperature of the stirring kettle is 100-120 ℃.
As a further improvement of the technical scheme of the invention, the stirring kettle in the fifth step is heated to 300-400 ℃ and the stirring speed is controlled to 600-800 r/min.
The invention has the beneficial effects that:
the prepared heat-conducting resin composition has good heat-conducting property, wherein the added aluminum oxide powder, boron nitride powder and graphite powder can effectively maintain high heat-conducting property, the added chlorinated paraffin has good flame retardant property, the flame retardant property and the adhesive property of the prepared heat-conducting resin composition can be improved, and the whole preparation process flow is simple, the preparation cost is low, the equipment requirement is low, and the operability is strong.
Detailed Description
The following description will clearly and fully describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
a thermally conductive resin composition capable of maintaining high thermal conductivity, characterized by comprising the following components in parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin.
And in this embodiment, specifically, it is: 20 parts of terephthalic acid, 2 parts of aluminum oxide, 5 parts of boron nitride, 2 parts of graphite, 1 part of deionized water, 3 parts of copper powder, 5 parts of ethylene glycol and 2 parts of chlorinated paraffin.
A method for producing a thermally conductive resin composition capable of maintaining high thermal conductivity, comprising the steps of:
step one, preparing raw materials, wherein the raw materials comprise the following parts by weight: 20 parts of terephthalic acid, 2 parts of aluminum oxide, 5 parts of boron nitride, 2 parts of graphite, 1 part of deionized water, 3 parts of copper powder, 5 parts of ethylene glycol and 2 parts of chlorinated paraffin;
grinding the solid powder, and sequentially placing aluminum oxide, boron nitride and graphite into a grinder to obtain aluminum oxide powder, boron nitride powder and graphite powder;
step three, preparing polyethylene glycol terephthalate, namely firstly synthesizing dihydroxyethyl terephthalate by esterification reaction of terephthalic acid and ethylene glycol, and then performing polycondensation reaction to prepare the polyethylene glycol terephthalate;
step four, preparing slurry, namely synchronously and slowly adding the alumina powder, the boron nitride powder and the graphite powder prepared in the step two into a stirring kettle, continuously stirring deionized water in the stirring kettle for 40 minutes after the three powders are uniformly mixed until the mixture in the stirring kettle is pasty, and obtaining the slurry;
step five, preparing a mixture, namely adding the polyethylene terephthalate prepared in the step three and the slurry prepared in the step four into the same stirring kettle, heating the stirring kettle, stirring for 5min, adding chlorinated paraffin into the stirring kettle, and continuously stirring for 30min to obtain a mixture;
and step six, molding, namely taking out the mixture prepared in the step five, placing the mixture into a glass container, and naturally cooling the mixture to obtain the heat-conducting resin composition.
As a further improvement of the technical scheme of the invention, in the second step, the grinding speed of the grinder is controlled to be 800r/min, the grinding time is controlled to be 30min, and the fineness of the solid powder obtained after grinding is controlled to be 200 meshes.
As a further improvement of the technical scheme of the invention, the polyethylene terephthalate prepared in the step three has the average molecular weight (2-3). Times.104, the glass transition temperature of 80 ℃, the Martin heat resistance of 80 ℃, the thermal deformation temperature of 98 ℃ (1.82 MPa) and the decomposition temperature of 353 ℃.
As a further improvement of the technical scheme of the invention, in the fourth step, the mixing time of the alumina powder, the boron nitride powder and the graphite powder in the stirring kettle is not less than 30min, the stirring speed is controlled to be 1200/min, and the internal temperature of the stirring kettle is 100 ℃.
As a further improvement of the technical scheme of the invention, in the fifth step, the temperature of the stirring kettle is raised to 300 ℃, and the stirring speed is controlled to be 600r/min.
Example 2:
a thermally conductive resin composition capable of maintaining high thermal conductivity, characterized by comprising the following components in parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin.
And in this embodiment, specifically, it is: 30 parts of terephthalic acid, 4 parts of aluminum oxide, 10 parts of boron nitride, 4 parts of graphite, 3 parts of deionized water, 5 parts of copper powder, 8 parts of ethylene glycol and 5 parts of chlorinated paraffin.
A method for producing a thermally conductive resin composition capable of maintaining high thermal conductivity, comprising the steps of:
step one, preparing raw materials, wherein the raw materials comprise the following parts by weight: 30 parts of terephthalic acid, 4 parts of aluminum oxide, 10 parts of boron nitride, 4 parts of graphite, 3 parts of deionized water, 5 parts of copper powder, 8 parts of ethylene glycol and 5 parts of chlorinated paraffin;
grinding the solid powder, and sequentially placing aluminum oxide, boron nitride and graphite into a grinder to obtain aluminum oxide powder, boron nitride powder and graphite powder;
step three, preparing polyethylene glycol terephthalate, namely firstly synthesizing dihydroxyethyl terephthalate by esterification reaction of terephthalic acid and ethylene glycol, and then performing polycondensation reaction to prepare the polyethylene glycol terephthalate;
step four, preparing slurry, namely synchronously and slowly adding the alumina powder, the boron nitride powder and the graphite powder prepared in the step two into a stirring kettle, continuously stirring deionized water in the stirring kettle for 60 minutes after the three powders are uniformly mixed until the mixture in the stirring kettle is pasty, and obtaining the slurry;
step five, preparing a mixture, namely adding the polyethylene terephthalate prepared in the step three and the slurry prepared in the step four into the same stirring kettle, heating the stirring kettle, stirring for 5min, adding chlorinated paraffin into the stirring kettle, and continuously stirring for 60min to obtain a mixture;
and step six, molding, namely taking out the mixture prepared in the step five, placing the mixture into a glass container, and naturally cooling the mixture to obtain the heat-conducting resin composition.
As a further improvement of the technical scheme of the invention, in the second step, the grinding speed of the grinder is controlled to be 600r/min, the grinding time is controlled to be 50min, and the fineness of the solid powder obtained after grinding is controlled to be 300 meshes.
As a further improvement of the technical scheme of the invention, the polyethylene terephthalate prepared in the step three has the average molecular weight (2-3). Times.104, the glass transition temperature of 80 ℃, the Martin heat resistance of 80 ℃, the thermal deformation temperature of 98 ℃ (1.82 MPa) and the decomposition temperature of 353 ℃.
As a further improvement of the technical scheme of the invention, in the fourth step, the mixing time of the alumina powder, the boron nitride powder and the graphite powder in the stirring kettle is not less than 30min, the stirring speed is controlled to be 1200r/min, and the internal temperature of the stirring kettle is 120 ℃.
As a further improvement of the technical scheme of the invention, in the fifth step, the temperature of the stirring kettle is raised to 400 ℃, and the stirring speed is controlled to be 800r/min.
Example 3:
a thermally conductive resin composition capable of maintaining high thermal conductivity, characterized by comprising the following components in parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin.
And in this embodiment, specifically, it is: 40 parts of terephthalic acid, 6 parts of aluminum oxide, 15 parts of boron nitride, 6 parts of graphite, 5 parts of deionized water, 8 parts of copper powder, 10 parts of ethylene glycol and 8 parts of chlorinated paraffin.
A method for producing a thermally conductive resin composition capable of maintaining high thermal conductivity, comprising the steps of:
step one, preparing raw materials, wherein the raw materials comprise the following parts by weight: 40 parts of terephthalic acid, 6 parts of aluminum oxide, 15 parts of boron nitride, 6 parts of graphite, 5 parts of deionized water, 8 parts of copper powder, 10 parts of ethylene glycol and 8 parts of chlorinated paraffin;
grinding the solid powder, and sequentially placing aluminum oxide, boron nitride and graphite into a grinder to obtain aluminum oxide powder, boron nitride powder and graphite powder;
step three, preparing polyethylene glycol terephthalate, namely firstly synthesizing dihydroxyethyl terephthalate by esterification reaction of terephthalic acid and ethylene glycol, and then performing polycondensation reaction to prepare the polyethylene glycol terephthalate;
step four, preparing slurry, namely synchronously and slowly adding the alumina powder, the boron nitride powder and the graphite powder prepared in the step two into a stirring kettle, continuously stirring deionized water in the stirring kettle for 60 minutes after the three powders are uniformly mixed until the mixture in the stirring kettle is pasty, and obtaining the slurry;
step five, preparing a mixture, namely adding the polyethylene terephthalate prepared in the step three and the slurry prepared in the step four into the same stirring kettle, heating the stirring kettle, stirring for 5min, adding chlorinated paraffin into the stirring kettle, and continuously stirring for 60min to obtain a mixture;
and step six, molding, namely taking out the mixture prepared in the step five, placing the mixture into a glass container, and naturally cooling the mixture to obtain the heat-conducting resin composition.
As a further improvement of the technical scheme of the invention, in the second step, the grinding speed of the grinder is controlled to be 800r/min, the grinding time is controlled to be 60min, and the fineness of the solid powder obtained after grinding is controlled to be 300 meshes.
As a further improvement of the technical scheme of the invention, the polyethylene terephthalate prepared in the step three has the average molecular weight (2-3). Times.104, the glass transition temperature of 80 ℃, the Martin heat resistance of 80 ℃, the thermal deformation temperature of 98 ℃ (1.82 MPa) and the decomposition temperature of 353 ℃.
As a further improvement of the technical scheme of the invention, in the fourth step, the mixing time of the alumina powder, the boron nitride powder and the graphite powder in the stirring kettle is not less than 30min, the stirring speed is controlled to 1500r/min, and the internal temperature of the stirring kettle is 120 ℃.
As a further improvement of the technical scheme of the invention, in the fifth step, the temperature of the stirring kettle is raised to 400 ℃, and the stirring speed is controlled to be 800r/min.
Three heat conductive resin compositions can be obtained through the above three groups of examples, and the three heat conductive resin compositions are respectively subjected to performance tests, so that the performance of the heat conductive resin compositions in the three groups of examples is improved differently, wherein the performance of the wall coating in the example 3 is the best, the value is the highest, and the obtained parameters are compared with the following table in the test process:
| thermal conductivity of | Flame retardant Properties | Adhesive properties | |
| Example 1 | Good quality | Good quality | High height |
| Example 2 | Good quality | Good quality | High height |
| Example 3 | High height | High height | High height |
From the above table, it can be seen that the thermal conductive resin composition prepared in the technical scheme has good thermal conductive performance, wherein the added aluminum oxide powder, boron nitride powder and graphite powder can effectively maintain high thermal conductive performance, the added chlorinated paraffin has good flame retardant performance, the flame retardant performance and the adhesive performance of the prepared thermal conductive resin composition can be improved, and the whole preparation process flow is simple, the preparation cost is low, the equipment requirement is low, and the operability is strong.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (8)
1. A thermally conductive resin composition capable of maintaining high thermal conductivity, characterized by comprising the following components in parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin.
2. The heat conductive resin composition as claimed in claim 1, which is capable of maintaining high heat conductivity, comprising the following components in parts by weight: 25-35 parts of terephthalic acid, 3-5 parts of aluminum oxide, 8-12 parts of boron nitride, 3-5 parts of graphite, 2-4 parts of deionized water, 4-6 parts of copper powder, 6-9 parts of ethylene glycol and 4-6 parts of chlorinated paraffin.
3. The heat conductive resin composition as claimed in claim 1, which is capable of maintaining high heat conductivity, comprising the following components in parts by weight: 30 parts of terephthalic acid, 4 parts of aluminum oxide, 10 parts of boron nitride, 4 parts of graphite, 3 parts of deionized water, 5 parts of copper powder, 8 parts of ethylene glycol and 5 parts of chlorinated paraffin.
4. A heat conductive resin composition capable of maintaining high heat conductivity according to claim 1 to 3, further comprising a process for producing a heat conductive resin composition capable of maintaining high heat conductivity, comprising the steps of:
step one, preparing raw materials, wherein the raw materials comprise the following parts by weight: 20-40 parts of terephthalic acid, 2-6 parts of aluminum oxide, 5-15 parts of boron nitride, 2-6 parts of graphite, 1-5 parts of deionized water, 3-8 parts of copper powder, 5-10 parts of ethylene glycol and 2-8 parts of chlorinated paraffin;
grinding the solid powder, and sequentially placing aluminum oxide, boron nitride and graphite into a grinder to obtain aluminum oxide powder, boron nitride powder and graphite powder;
step three, preparing polyethylene glycol terephthalate, namely firstly synthesizing dihydroxyethyl terephthalate by esterification reaction of terephthalic acid and ethylene glycol, and then performing polycondensation reaction to prepare the polyethylene glycol terephthalate;
step four, preparing slurry, namely synchronously and slowly adding the alumina powder, the boron nitride powder and the graphite powder prepared in the step two into a stirring kettle, continuously stirring deionized water in the stirring kettle for 40-60min after the three powders are uniformly mixed until the mixture in the stirring kettle is pasty, and obtaining the slurry;
step five, preparing a mixture, namely adding the polyethylene terephthalate prepared in the step three and the slurry prepared in the step four into the same stirring kettle, heating the stirring kettle, stirring for 5min, adding chlorinated paraffin into the stirring kettle, and continuously stirring for 30-60min to obtain a mixture;
and step six, molding, namely taking out the mixture prepared in the step five, placing the mixture into a glass container, and naturally cooling the mixture to obtain the heat-conducting resin composition.
5. The method for producing a heat conductive resin composition capable of maintaining high heat conductivity according to claim 4, characterized in that: in the second step, the grinding speed of the grinder is controlled to be 500-800r/min, the grinding time is controlled to be 30-60min, and the fineness of the solid powder obtained after grinding is controlled to be 200-300 meshes.
6. The method for producing a heat conductive resin composition capable of maintaining high heat conductivity according to claim 4, characterized in that: the polyethylene terephthalate prepared in the third step has an average molecular weight (2-3). Times.104, a glass transition temperature of 80 ℃, martin heat resistance of 80 ℃, a heat distortion temperature of 98 ℃ (1.82 MPa) and a decomposition temperature of 353 ℃.
7. The method for producing a heat conductive resin composition capable of maintaining high heat conductivity according to claim 4, characterized in that: in the fourth step, the mixing time of the alumina powder, the boron nitride powder and the graphite powder in the stirring kettle is not less than 30min, the stirring speed is controlled to be 1200-1500 r/min, and the temperature in the stirring kettle is 100-120 ℃.
8. The method for producing a heat conductive resin composition capable of maintaining high heat conductivity according to claim 4, characterized in that: and in the fifth step, the temperature of the stirring kettle is raised to 300-400 ℃, and the stirring speed is controlled to 600-800 r/min.
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