CN110734642A - insulating high-strength nano composite material and preparation method thereof - Google Patents
insulating high-strength nano composite material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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
- 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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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention discloses insulating high-strength nano composite materials, which are prepared from the following raw materials, by weight, 1) 1-10 parts of hydroxylated boron nitride/nylon 6 master batch, and 2) 6100 parts of nylon, wherein the composite material comprises a nylon 6 matrix and hydroxylated boron nitride, 50-70% of hydroxylated boron nitride is added into caprolactam through an in-situ polymerization method to carry out ring-opening polymerization of caprolactam, and the nylon is grafted onto the hydroxylated boron nitride through a grafting reaction with a surface functional group, so that the high-content hydroxylated boron nitride/nylon 6 master batch is prepared.
Description
Technical Field
The invention relates to the field of heat-conducting polymer composite materials, in particular to insulating high-strength nano composite materials and a preparation method thereof.
Background
With the high frequency and high speed of electronic devices and the rapid development of integrated circuit technology, the electronic devices have higher and higher requirements for heat dissipation, and rapid and effective heat diffusion becomes a very critical technology in material development. The high polymer is an ideal heat management material due to easy preparation, light weight and low cost,
nylon 6 has excellent mechanical properties, better electrical properties, wear resistance, oil resistance, solvent resistance, self-lubrication, corrosion resistance and good processing properties, is which is the largest variety among the current polyamide plastics and is widely applied to the fields of automobiles, electronic and electrical products, machinery and aerospace industry and daily life, but the structural characteristics of nylon 6 determine that the nylon 6 is a poor thermal conductor and limit the application of the nylon 6 in the field of heat conduction materials, the modification of nylon 6 by adopting heat conduction fillers is an effective way for improving the heat conductivity of nylon 6 and other high polymer materials, boron nitride is novel two-dimensional carbon nano materials, has a crystal structure similar to a graphite layer structure, has excellent electrical insulation, chemical stability and lower thermal expansion coefficient, shows excellent heat conductivity and is excellent heat conduction fillers.
Chinese patent application publication No. CN103450674A, " high thermal conductive nylon 6/graphene nanocomposite and a preparation method thereof", the method improves the dispersion degree of reduced graphene oxide in a nylon 6 matrix by functionalizing graphene and simultaneously adopting in-situ graft polymerization to reduce agglomeration, but the thermal conductive filler used in the method has excellent electrical conductivity and is not suitable for insulating materials, and meanwhile, the thermal conductive filler has a maximum addition amount of only 10%, so that the improvement of thermal conductivity is not obvious.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, insulating high-strength nano composite materials are provided, hexagonal boron nitride is functionalized, an in-situ grafting technology is adopted to enable a higher filler amount to enter a matrix, and high-filler amount boron nitride is uniformly dispersed in the matrix to significantly reduce interface thermal resistance, so that the heat conduction performance is significantly improved, and the composite materials have high insulating property and good mechanical property simultaneously,
the invention also provides methods for preparing the insulating high-strength nano composite material, which adopt easily available components, greatly reduce the cost of the composite material, have reasonable process and compact steps and are easy to industrialize.
In order to achieve the purpose, the invention adopts the following technical scheme:
kinds of insulated high-strength nano composite materials, which is characterized in that the insulated high-strength nano composite materials are prepared from the following raw materials in parts by weight:
1) 1-10 parts of hydroxylated boron nitride/nylon 6 master batch
2) 6100 portions of nylon.
The hydroxylated boron nitride/nylon 6 master batch is prepared from 50-70 parts by weight of hydroxylated boron nitride, 20-45 parts by weight of nylon 6 monomer and 1-5 parts by weight of catalyst or initiator through premixing, prepolymerization, polymerization, discharging, granulation, washing and drying.
The nylon 6 is pure polyamide 6.
The hydroxylated boron nitride is obtained by carrying out tip ultrasonic stripping on hexagonal boron nitride with the particle size of 4 microns, wherein the particle size is 400 nanometers, and the thickness is 5 nanometers.
The nylon 6 monomer is epsilon-caprolactam.
The catalyst or initiator is 6-aminocaproic acid or phosphoric acid.
the method for preparing the insulating high-strength nano composite material is characterized in that the in-situ grafting technology is adopted to uniformly disperse the high-filling boron nitride in the matrix so as to reduce the interface thermal resistance, and the method comprises the following steps:
(1) preparing hydroxylated boron nitride/nylon 6 master batch: adding 50-70% of hydroxylated boron nitride into caprolactam by an in-situ polymerization method, carrying out ring-opening polymerization on the caprolactam, and grafting nylon onto the hydroxylated boron nitride through a grafting reaction with a surface functional group, thereby preparing a high-content hydroxylated boron nitride/nylon 6 master batch;
(2) melt blending: and melting and blending the hydroxylated boron nitride/nylon 6 master batch and the nylon 6 in a set ratio in an internal mixer at 240-260 ℃, internally mixing and compounding for 1-4 hours, and discharging to obtain the insulating high-strength hydroxylated boron nitride/nylon 6 nano composite material.
The step (1) specifically comprises the following steps:
(11) preparing a hydroxylated boron nitride nanosheet: preparing a hydroxylated boron nitride nanosheet by taking hexagonal boron nitride as a raw material and adopting a tip ultrasonic technology through a solution exfoliation method: dispersing 1g of boron nitride powder in 100mL of 0.05 wt% sodium cholate aqueous solution, and performing tip ultrasonic treatment (600W,25 ℃) in an ultrasonic crusher for 10h to obtain 10 mg/mL-1Hydroxylated boron nitride nanoplates;
(12) preparing a premix: mixing a hydroxylated boron nitride monomer and a nylon 6 monomer with a catalyst or an initiator, and ultrasonically dispersing for 1-4 hours at 80-85 ℃ to form a premix;
(13) preparing a prepolymer: after the pre-mixture is dried for 1-3 hours in vacuum, pre-polymerizing for 1-4 hours at 160-200 ℃ under the protection of nitrogen to form a pre-polymer;
(14) polymerizing the prepolymer for 4-10 hours at 240-260 ℃ under the protection of nitrogen, and performing reduced pressure micromolecule removal operation 1-3 hours before the polymerization is finished, wherein the inside of the system is kept in vacuum;
(15) discharging under the protection of nitrogen, and granulating, washing and drying to obtain the hydroxylated boron nitride/nylon 6 master batch.
Compared with the prior art, the invention has the following beneficial effects:
(1) the insulating high-strength hydroxylated boron nitride/nylon 6 master batch adopted by the composite material has high content of the heat-conducting filler, and the covalent amide bond between the polymer matrix and the heat-conducting filler hydroxylated boron nitride is very tightly combined by adopting the heat-conducting master batch prepared by the covalent grafting technical strategy in the in-situ compounding method, so that the matrix-filler interface thermal resistance can be effectively reduced, and the heat conductivity of the composite material is improved.
(2) The preparation method provided by the invention has the advantages that the filler with higher content is more effectively and more uniformly dispersed in the matrix due to the bonding effect of amido bonds, and the insulating high-strength hydroxylated boron nitride/nylon 6 composite material can keep the good mechanical property of the polymer by a method of adding the filler into the pure nylon 6 matrix in a low master batch adding amount form.
(3) The insulating high-strength hydroxylated boron nitride/nylon 6 nano composite material provided by the invention has excellent heat-conducting property, low material cost, few preparation procedures, compact process and low cost, and can be used in heat dissipation fields of automobiles, computers, LEDs and the like.
Drawings
FIG. 1 is an SEM photograph of the insulating high-strength hydroxylated boron nitride/nylon 6 nanocomposite material of the invention.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention is further described with reference to the drawings.
Example 1: the embodiment of the invention provides an insulating high-strength nano composite material, which is prepared from the following raw materials in parts by weight:
1) 1-10 parts of hydroxylated boron nitride/nylon 6 master batch
2) 6100 portions of nylon.
The hydroxylated boron nitride/nylon 6 master batch is prepared from 50-70 parts by weight of hydroxylated boron nitride, 20-45 parts by weight of nylon 6 monomer and 1-5 parts by weight of catalyst or initiator through premixing, prepolymerization, polymerization, discharging, granulation, washing and drying.
The nylon 6 is pure polyamide 6.
The hydroxylated boron nitride is obtained by carrying out tip ultrasonic stripping on hexagonal boron nitride with the particle size of 4 microns, wherein the particle size is 400 nanometers, and the thickness is 5 nanometers.
The nylon 6 monomer is epsilon-caprolactam.
The catalyst or initiator is 6-aminocaproic acid or phosphoric acid.
the method for preparing the insulating high-strength nano composite material adopts the in-situ grafting technology to uniformly disperse the high-filling boron nitride in the matrix so as to reduce the interface thermal resistance, and comprises the following steps:
(1) preparing hydroxylated boron nitride/nylon 6 master batch: adding 50-70% of hydroxylated boron nitride into caprolactam by an in-situ polymerization method, carrying out ring-opening polymerization on the caprolactam, and grafting nylon onto the hydroxylated boron nitride through a grafting reaction with a surface functional group, thereby preparing a high-content hydroxylated boron nitride/nylon 6 master batch;
(2) melt blending: and melting and blending the hydroxylated boron nitride/nylon 6 master batch and the nylon 6 in a set ratio in an internal mixer at 240-260 ℃, internally mixing and compounding for 1-4 hours, and discharging to obtain the insulating high-strength hydroxylated boron nitride/nylon 6 nano composite material.
The step (1) specifically comprises the following steps:
(11) preparing a hydroxylated boron nitride nanosheet: preparing a hydroxylated boron nitride nanosheet by taking hexagonal boron nitride as a raw material and adopting a tip ultrasonic technology through a solution exfoliation method: dispersing 1g of boron nitride powder in 100mL of 0.05 wt% sodium cholate aqueous solution, and performing tip ultrasonic treatment (600W,25 ℃) in an ultrasonic crusher for 10h to obtain 10 mg/mL-1Hydroxylated boron nitride nanoplates;
(12) preparing a premix: mixing a hydroxylated boron nitride monomer and a nylon 6 monomer with a catalyst or an initiator, and ultrasonically dispersing for 1-4 hours at 80-85 ℃ to form a premix;
(13) preparing a prepolymer: after the pre-mixture is dried for 1-3 hours in vacuum, pre-polymerizing for 1-4 hours at 160-200 ℃ under the protection of nitrogen to form a pre-polymer;
(14) polymerizing the prepolymer for 4-10 hours at 240-260 ℃ under the protection of nitrogen, and performing reduced pressure micromolecule removal operation 1-3 hours before the polymerization is finished, wherein the inside of the system is kept in vacuum;
(15) discharging under the protection of nitrogen, and granulating, washing and drying to obtain the hydroxylated boron nitride/nylon 6 master batch.
Example 2:
the insulating high-strength nano composite material and the preparation method thereof provided by the embodiment of the invention are basically the same as the embodiment 1, and the difference is that:
preparation of hydroxylated boron nitride:
preparing the hydroxylated boron nitride nanosheet by a solution exfoliation method by adopting a tip ultrasonic technology. Dispersing 1g of boron nitride powder in 100mL of 0.05 wt% sodium cholate aqueous solution, and performing tip ultrasonic treatment (600W,25 ℃) in an ultrasonic crusher for 10h to obtain 10 mg/mL-1Hydroxylated boron nitride nanoplates.
Preparation of hydroxylated boron nitride/nylon 6 nanocomposite:
70 parts by weight of hydroxylated boron nitride, 27 parts by weight of epsilon-caprolactam and 3 parts by weight of 6-aminocaproic acid are mixed, intensively mixed by a physical method, and then ultrasonically dispersed for 3 hours at 80 ℃ to form a premix. The premix was dried under vacuum for 2 hours and prepolymerized at 180 ℃ under nitrogen for 2 hours. And polymerizing for 5 hours at 250 ℃ under the protection of nitrogen, finally discharging under the protection of nitrogen, and granulating, washing and drying to obtain the hydroxylated boron nitride/nylon 6 master batch.
Then mixing the hydroxylated boron nitride/nylon 6 master batch with 100 parts by weight of pure nylon 6 according to the formula in the table 1, carrying out melt blending and banburying compounding in a banbury mixer at 250 ℃ for 3 hours, and discharging to obtain the insulating high-strength boron nitride/nylon 6 nano composite materials with different addition amounts of the hydroxylated boron nitride.
Table 1: components and formulations of the examples
Table 2 shows that the performance of the composite material of the present invention (the filling amount of the hydroxylated boron nitride/nylon 6 is 10 wt%) is compared with the performance of the composite material in the prior art, and it can be seen from the table that the thermal conductivity and the insulation performance of the composite material of the present invention are significantly improved compared with those of the conventional material.
Table 2: the performance of the composite material of the invention is compared with that of the composite material in the prior art
The specific proportions of the components in the embodiments of the present invention can be selected within the ranges described according to specific needs, and the technical effects can be achieved, and the embodiments of the present invention are not listed in .
The invention is not limited to the above embodiment, and other insulated high-strength boron nitride/nylon 6 nano composite materials and preparation methods thereof, which are obtained by adopting the same or similar components, proportions and methods as those of the invention, are within the protection scope of the invention.
Claims (8)
1, kinds of insulating high-strength nano composite material, characterized in that, it is made up of following raw materials, it is counted according to the part by weight:
1) 1-10 parts of hydroxylated boron nitride/nylon 6 master batch
2) 6100 portions of nylon.
2. The insulating high-strength nanocomposite material as claimed in claim 1, wherein the hydroxylated boron nitride/nylon 6 masterbatch is prepared from 50-70 parts by weight of hydroxylated boron nitride, 20-45 parts by weight of nylon 6 monomer, and 1-5 parts by weight of catalyst or initiator by premixing, prepolymerization, polymerization, discharging, granulation, washing and drying.
3. The insulating nanocomposite of claim 1, wherein the nylon 6 is pure polyamide 6.
4. The insulated, high-strength nanocomposite material according to claim 2, wherein the hydroxylated boron nitride is obtained by subjecting hexagonal boron nitride having a particle size of 4 μm to tip ultrasonic exfoliation, the particle size being 400 nm and the thickness being 5 nm.
5. The insulated, high-strength nanocomposite material according to claim 2, wherein the nylon 6 monomer is epsilon-caprolactam.
6. The insulated, high-strength nanocomposite material according to claim 2, wherein the catalyst or initiator is 6-aminocaproic acid or phosphoric acid.
7, A method for preparing insulated high strength nanocomposite material as claimed in claims 1-6, wherein the method comprises the following steps:
(1) preparing hydroxylated boron nitride/nylon 6 master batch: adding 50-70% of hydroxylated boron nitride into caprolactam by an in-situ polymerization method, carrying out ring-opening polymerization on the caprolactam, and grafting nylon onto the hydroxylated boron nitride through a grafting reaction with a surface functional group, thereby preparing a high-content hydroxylated boron nitride/nylon 6 master batch;
(2) melt blending: and melting and blending the hydroxylated boron nitride/nylon 6 master batch and the nylon 6 in a set ratio in an internal mixer at 240-260 ℃, internally mixing and compounding for 1-4 hours, and discharging to obtain the insulating high-strength hydroxylated boron nitride/nylon 6 nano composite material.
8. The preparation method of the insulated high-strength nanocomposite material as claimed in claim 7, wherein the step (1) specifically comprises the following steps:
(11) preparing a hydroxylated boron nitride nanosheet: preparing a hydroxylated boron nitride nanosheet by taking hexagonal boron nitride as a raw material and adopting a tip ultrasonic technology through a solution exfoliation method: dispersing 1g of boron nitride powder in 100mL of 0.05wt% sodium cholate aqueous solution, and performing tip ultrasonic treatment (600W,25 ℃) in an ultrasonic crusher for 10 hours to obtain 10 mg/mL-1Hydroxylated boron nitride nanoplates;
(12) preparing a premix: mixing a hydroxylated boron nitride monomer and a nylon 6 monomer with a catalyst or an initiator, and ultrasonically dispersing for 1-4 hours at 80-85 ℃ to form a premix;
(13) preparing a prepolymer: after the pre-mixture is dried for 1-3 hours in vacuum, pre-polymerizing for 1-4 hours at 160-200 ℃ under the protection of nitrogen to form a pre-polymer;
(14) polymerizing the prepolymer for 4-10 hours at 240-260 ℃ under the protection of nitrogen, and performing reduced pressure micromolecule removal operation 1-3 hours before the polymerization is finished, wherein the inside of the system is kept in vacuum;
(15) discharging under the protection of nitrogen, and granulating, washing and drying to obtain the hydroxylated boron nitride/nylon 6 master batch.
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| CN114539766A (en) * | 2022-03-31 | 2022-05-27 | 上海天马微电子有限公司 | Flexible heat dissipation material, preparation method thereof and flexible display panel |
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