CN110734642B - 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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- 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
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Abstract
The invention discloses 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 composite material consists of a nylon 6 matrix and hydroxylated boron nitride, wherein the hydroxylated boron nitride with the content of 50-70 percent is added into caprolactam through an in-situ polymerization method to carry out ring-opening polymerization of the 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. The nano composite material provided by the invention has excellent heat conductivity and can be widely applied to the heat dissipation field of automobiles, computers, LEDs and the like. The invention also discloses a method for preparing the insulating high-strength nano composite material, which adopts an in-situ grafting technology to uniformly disperse high-filling boron nitride in a matrix so as to reduce the interface thermal resistance, and has reasonable preparation process and low comprehensive cost.
Description
Technical Field
The invention relates to the field of heat-conducting polymer composite materials, in particular to an insulating high-strength nano composite material 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,
the nylon 6 has excellent mechanical property, better electrical property, wear resistance, oil resistance, solvent resistance, self lubrication, corrosion resistance and good processing property, is one of the varieties with the largest output in the prior polyamide plastics, and is widely applied to the fields of automobiles, electronic and electric products, machinery, aerospace industry and daily life. However, the structural characteristics of nylon 6 determine that the nylon 6 is a poor thermal conductor, the application of the nylon 6 in the field of heat conduction materials is limited, and the modification of the nylon 6 by adopting the heat conduction filler is an effective way for improving the heat conductivity of the nylon 6 and other high polymer materials. Boron nitride is used as a novel two-dimensional carbon nano material, has a crystal structure similar to a graphite layer structure, has excellent electrical insulation, chemical stability and lower thermal expansion coefficient, shows excellent thermal conductivity and is an excellent heat-conducting filler.
Chinese patent application publication No. CN103450674A, "a high thermal conductivity 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 the improvement of thermal conductivity is not obvious. Chinese patent application publication No. CN10675177A, "a nylon 6-graphene master batch with heat conduction function and a preparation method thereof," the method directly performs melt extrusion on graphene and nylon 6 without in-situ polymerization and filler functionalization, so that the graphene is not uniformly dispersed in a matrix, the heat conduction performance improvement effect is not obvious, and the price of the graphene is high, which results in high overall material cost. Therefore, the novel composite material with good comprehensive performance, easy preparation and low cost is researched, and has great practical value.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide an insulating high-strength nano composite material, which is characterized in that hexagonal boron nitride is functionalized, an in-situ grafting technology is adopted to ensure that higher filler content enters a matrix, and the high-filler content boron nitride is uniformly dispersed in the matrix to obviously reduce interface thermal resistance, so that the heat conduction performance is obviously improved, and the composite material has high insulating property and good mechanical property; in addition to this, the present invention is,
the invention also provides a method for preparing the insulating high-strength nano composite material, which adopts easily obtained components and greatly reduces the cost of the composite material; the method has the advantages of reasonable process, compact steps and easy industrialization.
In order to achieve the purpose, the invention adopts the following technical scheme:
the insulated high-strength nano composite material is characterized by being 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 an in-situ grafting technology is adopted to uniformly disperse high-filling boron nitride in a 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 nitrogen hydroxide by using hexagonal boron nitride as raw material and adopting tip ultrasonic technology through solution exfoliation methodBoron nano-sheet: 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 widely applied to the heat-radiating 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 below with reference to the accompanying 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.
A method for preparing the insulating high-strength nano composite material adopts an in-situ grafting technology to uniformly disperse high-filling boron nitride in a 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 invention can be selected within the recorded ranges according to specific needs, and the technical effects can be achieved.
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 (3)
1. The insulated high-strength nano composite material is characterized by being 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 by 50-70 parts of hydroxylated boron nitride, 20-45 parts of nylon 6 monomer and 1-5 parts of catalyst or initiator by weight part 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.
2. A method for preparing the insulating high-strength nano composite material as claimed in claim 1, wherein an in-situ grafting technology is adopted to uniformly disperse high-filling boron nitride in a 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 through 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.
3. The preparation method of the insulated high-strength nanocomposite material as claimed in claim 2, 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 0.05 wt% sodium cholate aqueous solution, and carrying out tip ultrasonic treatment 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.
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| CN113061246A (en) * | 2021-03-26 | 2021-07-02 | 江苏苏能新材料科技有限公司 | Preparation method of high-fluidity heat-conducting nylon 6 master batch |
| CN113024801A (en) * | 2021-03-26 | 2021-06-25 | 江苏苏能新材料科技有限公司 | Rotational molding preparation method of high-thermal-conductivity nylon 6 hollow part |
| CN114539766B (en) * | 2022-03-31 | 2024-06-14 | 上海天马微电子有限公司 | Flexible heat dissipation material, preparation method thereof and flexible display panel |
| CN116217951A (en) * | 2022-12-22 | 2023-06-06 | 中国科学院福建物质结构研究所 | High-heat-conductivity powder with thermoplastic property and preparation method and application thereof |
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