CN112111134A - High-thermal-conductivity polyester material, preparation method thereof and high-thermal-conductivity biaxially oriented polyester film - Google Patents
High-thermal-conductivity polyester material, preparation method thereof and high-thermal-conductivity biaxially oriented polyester film Download PDFInfo
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- CN112111134A CN112111134A CN202010869871.2A CN202010869871A CN112111134A CN 112111134 A CN112111134 A CN 112111134A CN 202010869871 A CN202010869871 A CN 202010869871A CN 112111134 A CN112111134 A CN 112111134A
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy 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
- 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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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a high-thermal-conductivity polyester material which comprises the following raw materials: polyester resin and boron nitride particles, wherein the content of the boron nitride particles is 4-8 wt%, and the particle diameter of the boron nitride particles is 2-10 μm and 200-800 nm. The invention also discloses a preparation method of the high-thermal-conductivity polyester material. The invention also discloses a high-thermal-conductivity biaxially oriented polyester film which comprises the following raw materials: polyethylene terephthalate and the high thermal conductive polyester material. The invention has good heat-conducting property.
Description
Technical Field
The invention relates to the technical field of plastic films, in particular to a high-thermal-conductivity polyester material, a preparation method thereof and a high-thermal-conductivity biaxially oriented polyester film.
Background
Along with the high integration and miniaturization development of electric products such as electronic components, motors and the like, the heat per unit area is greatly increased, and the service life of the electric products is obviously shortened. In order to reduce the heat generation, a material with high heat conductivity must be used to lead out the heat generated by the operation of the electric appliance in time.
In the field of flexible electronics, a heat-resistant film is often used as a base film or a cover film of a flexible circuit for supporting and protecting the circuit, and the circuit generates heat during working, so that the film is required to have certain heat resistance and heat conductivity, and can effectively transfer heat and dissipate heat so as to eliminate the problem of heat generation caused by high circuit integration level.
In the high-end electronic field, a polyimide film having high thermal conductivity is generally used as a base film or a cover film of a flexible circuit, and in a field where requirements are not particularly severe, a polyester film may be used instead of an expensive polyimide film.
The biaxially oriented polyethylene terephthalate (BOPET) film has certain heat resistance, the BOPET film can endure the temperature of 120 ℃ and 150 ℃, although the heat resistance of the BOPET film can not reach the polyimide film, the BOPET film can meet the requirements of part of low-end electrical and electronic fields. However, the BOPET film has a thermal conductivity of about 0.18W/(m.k), and thus has poor thermal conductivity.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-thermal-conductivity polyester material, a preparation method thereof and a high-thermal-conductivity biaxially oriented polyester film, and the high-thermal-conductivity biaxially oriented polyester film has good thermal conductivity.
The invention provides a high-thermal-conductivity polyester material which comprises the following raw materials: polyester resin and boron nitride particles, wherein the content of the boron nitride particles is 4-8 wt%, and the particle diameter of the boron nitride particles is 2-10 μm and 200-800 nm.
Polyester is a generic term for polymers obtained by polycondensation of polyhydric alcohols and polybasic acids; mainly polyethylene terephthalate (PET), and conventionally includes linear thermoplastic resins such as polybutylene terephthalate (PBT) and polyarylate. The polyester material includes polyester resin and polyester elastomer. The polyester resin in turn includes polyethylene terephthalate (PET), polybutylene terephthalate (PBT), Polyarylate (PAR), and the like.
Preferably, the weight ratio of the boron nitride particles with the particle size of 2-10 μm to the boron nitride particles with the particle size of 200-800nm is 1: 3-10.
Preferably, the boron nitride particles are one of hexagonal boron nitride, a mixture of hexagonal boron nitride and a substance a, wherein the substance a is at least one of beryllium oxide, aluminum nitride, magnesium oxide, aluminum oxide and silicon nitride.
The invention also provides a preparation method of the high-thermal-conductivity polyester material, which comprises the following steps:
s1, uniformly mixing the dispersing agent, the boron nitride particles and ethylene glycol, adjusting the pH value to 2-3, heating to 90-110 ℃, keeping the temperature, stirring for 1-2h, and performing ultrasound treatment for 2-3h to obtain a boron nitride suspension;
s2, uniformly mixing the dibasic acid, the dihydric alcohol, the catalyst and the boron nitride suspension, carrying out esterification reaction in an inert gas atmosphere, then vacuumizing, and carrying out polycondensation reaction to obtain the high-thermal-conductivity polyester material.
The dibasic acid, the dihydric alcohol and the catalyst are common raw materials for preparing the polyester resin, and a person skilled in the art can select a suitable substance from a plurality of dibasic acids, dihydric alcohols and catalysts, such as: terephthalic acid, ethylene glycol, antimony trioxide, and the like.
Preferably, in S1, the content of the boron nitride particles in the boron nitride suspension is 0.05 to 0.1 wt%.
Preferably, in S1, the stirring speed is 1000-1800 r/min.
Preferably, in S1, the pH is adjusted with acetic acid.
Preferably, in S1, the dispersant is ammonium polyacrylate or sodium isobutyl sulfonate.
Preferably, in S1, the weight ratio of the dispersant to the ethylene glycol is 1: 4000-9000.
Preferably, in S2, the esterification reaction temperature is 220-270 ℃ and the esterification reaction time is 3-4 h.
Preferably, in S2, the polycondensation reaction temperature is 265-290 ℃ and the polycondensation reaction time is 3-5 h.
Preferably, in S2, after evacuation, the pressure is 30-50 Pa.
The high-thermal-conductivity polyester material can be prepared into the high-thermal-conductivity polyester master batch through filament making, cooling, cutting and granulation.
The invention also provides a high-thermal-conductivity biaxially oriented polyester film which comprises the following raw materials: polyethylene terephthalate and the high thermal conductive polyester material.
Preferably, the content of the high thermal conductive polyester material is 40 to 50 wt%.
The high-thermal-conductivity biaxially oriented polyester film can be a single-layer film or a multi-layer film, such as 3 layers; the thickness may be 12-25 μm.
Has the advantages that:
according to the invention, by introducing a proper amount of micron-scale and nano-scale boron nitride particles into the polyester resin, on one hand, micron boron nitride particles are contacted with each other to form a heat conduction network, on the other hand, the nano boron nitride is utilized to increase the contact area between the micron boron nitride particles, so that the heat conduction performance is improved, the heat conduction coefficient of the prepared polyester film is about 0.8W/(m.k), and the polyester film has good heat conduction performance; the addition amount of the boron nitride particles is less than that of single micron-scale or nano-scale boron nitride particles; the problems that a filter screen is easy to block when a melt is filtered, the surface of the film is not smooth, bubbles, needle holes and the like in the process of preparing the film due to the addition of single micron-sized boron nitride particles can be avoided; the problems that single nanometer-scale boron nitride particles are added, the boron nitride particles are easy to agglomerate and the transparency of the film is greatly reduced can be avoided.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A high heat conduction polyester material comprises the following raw materials: the polyester resin comprises 4 wt% of hexagonal boron nitride, the particle size of the hexagonal boron nitride is 2-10 mu m and 200-800nm, and the weight ratio of the hexagonal boron nitride with the particle size of 2-10 mu m to the hexagonal boron nitride with the particle size of 200-800nm is 1: 3.
The preparation method of the high-thermal-conductivity polyester material comprises the following steps:
s1, mixing ammonium polyacrylate, hexagonal boron nitride and ethylene glycol uniformly, adjusting the pH value to 2.5 by using acetic acid, heating to 100 ℃, stirring at 1400r/min for 1.5h under heat preservation, and performing ultrasonic treatment for 2.5h to obtain a boron nitride suspension with the hexagonal boron nitride content of 0.07 wt%, wherein the weight ratio of the ammonium polyacrylate to the ethylene glycol is 1: 7000;
s2, uniformly mixing terephthalic acid, ethylene glycol, antimony trioxide and boron nitride suspension, carrying out esterification reaction for 3.5h at 250 ℃ under the protection of nitrogen, then carrying out vacuum pumping until the pressure is 40Pa, carrying out polycondensation reaction for 4h at 275 ℃ to obtain a high-thermal-conductivity polyester material, and carrying out yarn making, cooling, cutting and granulation to obtain the high-thermal-conductivity polyester master batch.
Example 2
A high heat conduction polyester material comprises the following raw materials: the polyester resin and the boron nitride particles, wherein the content of the boron nitride particles is 6 wt%, the particle diameters of the boron nitride particles are 2-10 mu m and 200-800nm, and the weight ratio of the boron nitride particles with the particle diameters of 2-10 mu m to the boron nitride particles with the particle diameters of 200-800nm is 1: 10;
the boron nitride particles are a mixture of hexagonal boron nitride and alumina, wherein the weight ratio of hexagonal boron nitride to alumina is 4: 1.
The preparation method of the high-thermal-conductivity polyester material comprises the following steps:
s1, mixing sodium isobutyl sulfonate, boron nitride particles and ethylene glycol uniformly, adjusting the pH value to 2 by using acetic acid, heating to 110 ℃, keeping the temperature at 1000r/min, stirring for 2 hours, and performing ultrasonic treatment for 2 hours to obtain a boron nitride suspension with the boron nitride particle content of 0.1 wt%, wherein the weight ratio of the sodium isobutyl sulfonate to the ethylene glycol is 1: 4000;
s2, uniformly mixing terephthalic acid, ethylene glycol, antimony trioxide and boron nitride suspension, carrying out esterification reaction for 3h at 270 ℃ under the protection of nitrogen, then vacuumizing until the pressure is 50Pa, carrying out polycondensation reaction for 5h at 265 ℃ to obtain a high-thermal-conductivity polyester material, and carrying out yarn making, cooling, cutting and granulation to obtain the high-thermal-conductivity polyester master batch.
Example 3
A high heat conduction polyester material comprises the following raw materials: the polyester resin comprises 8 wt% of hexagonal boron nitride, the particle size of the hexagonal boron nitride is 2-10 mu m and 200-800nm, and the weight ratio of the hexagonal boron nitride with the particle size of 2-10 mu m to the hexagonal boron nitride with the particle size of 200-800nm is 1: 3.
The preparation method of the high thermal conductivity polyester material is the same as that of the embodiment 1.
Comparative example 1
The particle size of hexagonal boron nitride is 2-10 μm, and the high thermal conductivity polyester master batch is prepared by the same method as the embodiment 1.
Comparative example 2
The particle size of the hexagonal boron nitride is 200-800nm, and the high thermal conductivity polyester master batch is prepared by the method in the same way as the example 1.
Comparative example 3
A polyester masterbatch was prepared without hexagonal boron nitride, otherwise as in example 1.
Test examples
Single-layer biaxially oriented polyester films having a thickness of 20 μm were prepared in the same manner by mixing examples 1 to 3 and comparative examples 1 to 3 with polyethylene terephthalate, respectively (wherein the content of the polyester master batch obtained in examples 1 to 3 and comparative examples 1 to 3 was 40% by weight), and the properties of the films were measured, respectively, as shown in the following tables:
the above table shows that the heat conductivity coefficient of the film can be obviously improved after the boron nitride particles are added, the micron-scale and nano-scale boron nitride particles can better improve the heat conduction effect under the same addition amount, and meanwhile, the mechanical property and the optical property of the film cannot be obviously reduced on the premise of achieving the heat conduction effect.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The high-thermal-conductivity polyester material is characterized by comprising the following raw materials: polyester resin and boron nitride particles, wherein the content of the boron nitride particles is 4-8 wt%, and the particle diameter of the boron nitride particles is 2-10 μm and 200-800 nm.
2. The polyester material with high thermal conductivity as claimed in claim 1, wherein the weight ratio of the boron nitride particles with particle size of 2-10 μm to the boron nitride particles with particle size of 200-800nm is 1: 3-10.
3. The polyester material of claim 1 or 2, wherein the boron nitride particles are hexagonal boron nitride, or a mixture of hexagonal boron nitride and a substance A, wherein the substance A is at least one of beryllium oxide, aluminum nitride, magnesium oxide, aluminum oxide, and silicon nitride.
4. A method for preparing the high thermal conductive polyester material according to any one of claims 1 to 3, comprising the steps of:
s1, uniformly mixing the dispersing agent, the boron nitride particles and ethylene glycol, adjusting the pH value to 2-3, heating to 90-110 ℃, keeping the temperature, stirring for 1-2h, and performing ultrasound treatment for 2-3h to obtain a boron nitride suspension;
s2, uniformly mixing the dibasic acid, the dihydric alcohol, the catalyst and the boron nitride suspension, carrying out esterification reaction in an inert gas atmosphere, then vacuumizing, and carrying out polycondensation reaction to obtain the high-thermal-conductivity polyester material.
5. The method for preparing a highly thermally conductive polyester material as claimed in claim 4, wherein the content of the boron nitride particles in the boron nitride suspension is 0.05 to 0.1 wt% in S1.
6. The method for preparing the polyester material with high thermal conductivity as claimed in claim 4 or 5, wherein in S1, the stirring speed is 1800 r/min; preferably, in S1, the pH is adjusted with acetic acid.
7. The method for preparing a high thermal conductive polyester material according to any one of claims 4 to 6, wherein in S1, the dispersant is ammonium polyacrylate or sodium isobutyl sulfonate; preferably, in S1, the weight ratio of the dispersant to the ethylene glycol is 1: 4000-9000.
8. The method for preparing the polyester material with high thermal conductivity according to any one of claims 4 to 7, wherein in S2, the esterification reaction temperature is 220 ℃ and 270 ℃, and the esterification reaction time is 3-4 h; preferably, in S2, the polycondensation reaction temperature is 265-290 ℃, and the polycondensation reaction time is 3-5 h; preferably, in S2, after evacuation, the pressure is 30-50 Pa.
9. The high-thermal-conductivity biaxially oriented polyester film is characterized by comprising the following raw materials: polyethylene terephthalate and a highly thermally conductive polyester material according to any of claims 1 to 3.
10. The biaxially oriented polyester film of claim 9, wherein the content of the high thermal conductive polyester material is 40 to 50 wt%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010869871.2A CN112111134A (en) | 2020-08-26 | 2020-08-26 | High-thermal-conductivity polyester material, preparation method thereof and high-thermal-conductivity biaxially oriented polyester film |
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| CN202010869871.2A CN112111134A (en) | 2020-08-26 | 2020-08-26 | High-thermal-conductivity polyester material, preparation method thereof and high-thermal-conductivity biaxially oriented polyester film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115709595A (en) * | 2022-11-04 | 2023-02-24 | 宁波东旭成新材料科技有限公司 | Heat conduction reflective film |
| CN116589864A (en) * | 2023-05-22 | 2023-08-15 | 苏州博濬新材料科技有限公司 | Preparation method of heat-conductive resin composition capable of maintaining high heat conductivity |
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| CN102766251A (en) * | 2012-07-31 | 2012-11-07 | 华润包装材料有限公司 | Quick-heat-absorbing polyester and preparation method thereof |
| CN104788911A (en) * | 2015-04-29 | 2015-07-22 | 华中科技大学 | Epoxy resin composite material, preparation method and application |
| CN105111900A (en) * | 2015-09-18 | 2015-12-02 | 深圳市莱特宁新材料科技有限公司 | Coating with high thermal conductivity and insulating performance, and preparation method and application of coating |
| CN110055020A (en) * | 2019-05-16 | 2019-07-26 | 魏月秀 | A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient |
-
2020
- 2020-08-26 CN CN202010869871.2A patent/CN112111134A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766251A (en) * | 2012-07-31 | 2012-11-07 | 华润包装材料有限公司 | Quick-heat-absorbing polyester and preparation method thereof |
| CN104788911A (en) * | 2015-04-29 | 2015-07-22 | 华中科技大学 | Epoxy resin composite material, preparation method and application |
| CN105111900A (en) * | 2015-09-18 | 2015-12-02 | 深圳市莱特宁新材料科技有限公司 | Coating with high thermal conductivity and insulating performance, and preparation method and application of coating |
| CN110055020A (en) * | 2019-05-16 | 2019-07-26 | 魏月秀 | A kind of epoxy pouring sealant and preparation method of high thermal conductivity coefficient |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115709595A (en) * | 2022-11-04 | 2023-02-24 | 宁波东旭成新材料科技有限公司 | Heat conduction reflective film |
| CN116589864A (en) * | 2023-05-22 | 2023-08-15 | 苏州博濬新材料科技有限公司 | Preparation method of heat-conductive resin composition capable of maintaining high heat conductivity |
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Application publication date: 20201222 |