CN111286081A - Aluminum nitride compound, flame-retardant material containing compound and preparation method - Google Patents
Aluminum nitride compound, flame-retardant material containing compound and preparation method Download PDFInfo
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Abstract
The invention relates to the field of flame-retardant materials, in particular to an aluminum nitride compound, a flame-retardant material containing the compound and a preparation method of the flame-retardant material. The aluminum nitride composite provided by the invention comprises: 80-120 parts of aluminum nitride, 0.5-2 parts of a first coupling agent, 30-50 parts of a polyolefin elastomer, 0.8-2 parts of maleic anhydride and 0.1-1 part of dicumyl peroxide. The invention provides a polyamide flame-retardant material, which comprises: 31-62 parts of polyamide, 5-10 parts of a flame retardant, 2-4 parts of a synergistic flame retardant, 30-50 parts of a heat-conducting filler, 5-20 parts of glass fiber, 1-10 parts of an aluminum nitride compound, 0.1-5 parts of a lubricant and 0-2 parts of a second coupling agent; the components have synergistic effect. The experimental result shows that the self-made aluminum nitride compound is introduced, so that the heat conductivity coefficient and the toughness of the material are obviously improved, and the material has high practical value.
Description
Technical Field
The invention relates to the technical field of flame-retardant materials, in particular to an aluminum nitride compound, a flame-retardant material containing the compound and a preparation method of the flame-retardant material.
Background
With the rapid development of fifth generation mobile communication networks (5G networks for short), the large-scale commercialization of 5G networks has been in the forefront. The working frequency band of the 5G network is far higher than that of the 4G network, and the heat generated by the base station equipment during working is far higher than that of the 4G network; in addition, in recent years, portable and lightweight electronic equipment is developed rapidly, the performance and the assembly density of electronic devices are improved, and the heat generation amount is improved, so that higher requirements on the heat conductivity and the mechanical property of the polyamide material are provided.
Polyamide composite materials are widely used in the fields of electronics, electrical and mechanical equipment, etc. because of their excellent heat resistance. In the conventional technology, the main means for improving the thermal conductivity of polyamide is to fill a polyamide matrix with a thermal conductive filler. Most of the heat-conducting fillers commonly used in the prior art are inorganic metal-nonmetal compounds, but in actual production, the following limitations exist: more heat-conducting fillers are often required to be added when higher heat-conducting performance is required to be obtained, but the compatibility of the inorganic heat-conducting fillers and the organic polymer material matrix is poor, and the mechanical performance of the composite material is obviously reduced due to excessive addition of the heat-conducting fillers; in addition, excessive addition of the heat-conducting filler can generate a large number of interfaces in the composite material, and the interfaces can block the transmission of heat in the material, so that the heat conductivity coefficient of the material is not obviously increased. Therefore, the compatibility of the inorganic heat-conducting filler and the polymer matrix is enhanced, the interface between the inorganic heat-conducting filler and the polymer matrix is reduced, the heat-conducting coefficient can be effectively improved, the reduction of the mechanical property can be avoided, and moreover, the material can have higher heat-conducting coefficient when less heat-conducting filler is added, and the using amount of the heat-conducting filler is reduced.
Disclosure of Invention
In view of this, it is necessary to provide a material having a heat conductive function that can be well compatible with a polymer matrix, in order to solve the problem of poor compatibility between a heat conductive filler and an organic polymer material matrix.
The invention aims to provide an aluminum nitride compound and a preparation method thereof. The aluminum nitride compound has good compatibility with a polymer matrix material and has good heat conduction effect.
The invention also aims to provide a polyamide flame-retardant material containing the aluminum nitride compound and a preparation method thereof.
Specifically, the aluminum nitride composite is prepared by compounding aluminum nitride and a polyolefin elastomer in advance, and the polyolefin elastomer is used for enhancing the compatibility between the aluminum nitride composite and a polymer matrix, so that the thermal conductivity of the polymer composite is remarkably improved, and the mechanical property of the polymer composite is enhanced. Meanwhile, the aluminum nitride has better thermal conductivity, can replace heat-conducting fillers to a certain extent, and can reduce the dosage of the heat-conducting fillers in the polyamide flame-retardant material by introducing the aluminum nitride, thereby avoiding the problem of reduced mechanical properties caused by adding excessive heat-conducting fillers.
The invention provides an aluminum nitride compound, which comprises the following components in parts by weight:
in one embodiment, the grain size of the aluminum nitride is 1-100 μm.
In one embodiment, the first coupling agent is at least one of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent, and a chromium complex coupling agent.
The invention also provides a preparation method of the aluminum nitride compound, which comprises the following steps:
preparing materials according to the proportion of the raw materials in the aluminum nitride compound, fully mixing the aluminum nitride and the first coupling agent, adding the polyolefin elastomer, the maleic anhydride and the dicumyl peroxide, banburying, extruding and granulating.
In one embodiment, the banburying temperature is 150-200 ℃, the rotating speed is 30-60 r/min, and the time is 3-10 min.
In one embodiment, the extrusion granulation is carried out by adopting a single-screw extruder, the extrusion temperature is 160-180 ℃, and the screw rotation speed is 70-150 r/min.
The invention also provides a flame-retardant material which comprises the aluminum nitride compound.
Specifically, the composition comprises the following components in parts by weight:
in one embodiment, the polyamide is selected from at least one of polycaprolactam and polyhexamethylene adipamide.
In one embodiment, the viscosity coefficient of the polyamide is 2.0-4.5.
In one embodiment, the flame retardant is a brominated flame retardant. Specifically, the flame retardant is selected from at least one of decabromodiphenyl ether, tetrabromobisphenol A, octabromoether, brominated polystyrene, decabromodiphenyl ethane, and brominated epoxy resin.
In one embodiment, the synergistic flame retardant is an antimonide. Specifically, the synergistic flame retardant is selected from at least one of sodium antimonate, antimony pentoxide and antimony trioxide.
In one embodiment, the thermally conductive filler is selected from at least one of magnesium oxide, aluminum oxide, magnesium hydroxide, aluminum hydroxide, magnesium nitride, aluminum nitride, and boron nitride.
In one embodiment, the glass fibers are milled alkali-free glass fibers having a length of 50 μm to 210 μm.
In one embodiment, the lubricant is at least one of silicone powder, ethylene bis stearamide, and calcium stearate.
In one embodiment, the second coupling agent is a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent, and a chromium complex coupling agent.
The invention also provides a preparation method of the flame-retardant material, which comprises the following steps:
and mixing the polyamide, the flame retardant, the synergistic flame retardant, the heat-conducting filler, the glass fiber, the aluminum nitride compound, the lubricant and the second coupling agent, and then extruding and granulating.
In one embodiment, the extrusion granulation process is carried out by adopting a double-screw extruder, wherein the temperature of a first zone of the double-screw extruder is 200-210 ℃, the temperature of a second zone of the double-screw extruder is 220-250 ℃, the temperature of a third zone of the double-screw extruder is 240-250 ℃, the temperature of a fourth zone of the double-screw extruder is 240-250 ℃, the temperature of a machine head of the double-screw extruder is 250-260 ℃, the total residence time is 1-2 min, and the pressure is.
The aluminum nitride compound provided by the invention is prepared by preparing the aluminum nitride, the polyolefin elastomer and other additives into a composite material in advance, has the high thermal conductivity of the aluminum nitride and the high toughness of the polyolefin elastomer, and can improve the thermal conductivity and the mechanical property of a high polymer material by taking the aluminum nitride as an additive material. In addition, the polyolefin elastomer can also enhance the compatibility between the aluminum nitride compound and the polymer matrix, effectively solves the problem of poor compatibility between the heat-conducting filler and the polymer matrix, and has practical value.
The polyamide flame-retardant material containing the aluminum nitride compound has excellent heat-conducting property and mechanical property. Moreover, experiments prove that the aluminum nitride compound can replace a part of heat-conducting filler in the polyamide flame-retardant material, the using amount of the inorganic heat-conducting filler is obviously reduced on the premise of keeping the excellent heat-conducting property of the flame-retardant material, and the problem of poor mechanical property caused by excessive addition of the inorganic heat-conducting filler is avoided.
Detailed Description
In order that the manner in which the above recited features and objects of the present invention are obtained will be readily understood, a more complete description of the invention briefly summarized above may be had by reference to the embodiments thereof which are illustrated in the appended drawings. The preferred embodiments of the present invention are given in the examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
One embodiment of the invention provides an aluminum nitride composite, which comprises the following components in parts by weight:
preferably, the aluminum nitride compound comprises the following components in parts by weight:
as a specific example, the particle size of aluminum nitride is 1 μm to 100. mu.m. The aluminum nitride can play a role in heat conduction in the aluminum nitride compound, and the heat conductivity of the composite material is enhanced. The reason for selecting aluminum nitride for the composite is that the coefficient of thermal conductivity of aluminum nitride in the commonly used heat-conducting filler is relatively high and reaches 209W/m.K. While materials with higher thermal conductivity, such as silicon carbide, can achieve a thermal conductivity of 256W/m.K, they are green and not conducive to the production of white articles.
As a specific example, the polyolefin elastomer is a base material of an aluminum nitride composite, which can enhance the compatibility of the composite material with other polymer base materials, and the better toughness of the polyolefin elastomer can also improve the toughness of the final composite material as a whole.
As a specific example, the first coupling agent is at least one of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent, and a chromium complex coupling agent. Preferably, the first coupling agent is a silane coupling agent. The first coupling agent can improve the brightness of the surface of the product, improve the compatibility of an organic matrix and an inorganic substance and improve the comprehensive mechanical property of the composite material.
The aluminum nitride composite can be prepared according to the following method:
the materials are prepared according to the proportion of the raw materials in the aluminum nitride compound in the embodiment, the aluminum nitride and the coupling agent are fully mixed, then the polyolefin elastomer, the maleic anhydride and the dicumyl peroxide are added, and extrusion granulation is carried out after banburying.
As a specific example, the temperature of banburying is 150-200 ℃, the rotating speed is 30-60 r/min, and the time is 3-10 min. Preferably, the banburying temperature is 180 ℃ and the banburying time is 5 min.
As a specific example, the extrusion granulation is carried out by adopting a single-screw extruder, the extrusion temperature is 160-180 ℃, and the screw rotation speed is 70-150 r/min. Preferably, the extrusion temperature is 170 ℃.
The aluminum nitride compound prepared by the process has the high thermal conductivity and the high toughness of the aluminum nitride and the polyolefin elastomer, and is easy to compound with other polymer matrix materials to improve the thermal conductivity and the mechanical property of the aluminum nitride compound. The aluminum nitride compound taking the polyolefin elastomer as the matrix has better compatibility with the polymer matrix material, and avoids the reduction of mechanical property caused by poor compatibility. Moreover, the aluminum nitride compound has a heat conduction function, can replace a part of heat conduction filler, and further effectively reduces the using amount of the heat conduction filler.
The embodiment of the invention further provides a polyamide flame-retardant material containing the aluminum nitride compound, which comprises the following raw material components in parts by weight:
more specifically, the polyamide flame retardant material comprises the following raw material components in parts by weight:
as a specific example, the polyamide is at least one selected from polycaprolactam and polyhexamethylene adipamide, and the viscosity coefficient of the polyamide is 2.0 to 4.5. Polyamide is the base material of the composite.
As a specific example, the flame retardant is a bromine-based flame retardant, and more specifically, may be at least one of decabromodiphenyl ether, tetrabromobisphenol a, octabromoether, brominated polystyrene, decabromodiphenyl ethane, and brominated epoxy resin. The active ingredient of the flame retardant is bromine, and the flame retardant can play a role in high-efficiency flame retardance.
As a specific example, the synergistic flame retardant is an antimonide, and more specifically, may be at least one of sodium antimonate, antimony pentoxide, and antimony trioxide. The antimonide as the synergistic flame retardant has the effective component of antimony element, and can perform synergistic action with bromine element in the brominated flame retardant to play a role in high-efficiency flame retardance.
As a specific example, the thermally conductive filler is selected from at least one of magnesium oxide, aluminum oxide, magnesium hydroxide, aluminum hydroxide, magnesium nitride, aluminum nitride, and boron nitride. The inorganic heat-conducting filler has high heat conductivity coefficient, and can be added into the polymer matrix to effectively improve the heat conductivity coefficient of the composite material, but the compatibility of the inorganic heat-conducting filler and the polymer matrix is poor, a large number of interfaces exist in the composite material, and the interfaces not only can cause the reduction of the mechanical property of the composite material, but also can hinder the conduction of heat in the material and hinder the improvement of the heat conductivity coefficient of the composite material. Therefore, the excessive addition of the heat-conducting filler can not obviously improve the heat conductivity coefficient of the composite material, and can also reduce the mechanical property of the material.
The aluminum nitride compound provided by the invention is an additive which can effectively solve the problems.
As a specific example, the glass fibers are milled alkali-free glass fibers having a length of 50 μm to 210 μm. The glass fiber has high strength, and can effectively enhance the mechanical property of the composite material by using the glass fiber as an additive of a polyamide material.
As a specific example, the lubricant is at least one of silicone powder, ethylene-based bis-stearamide, and calcium stearate. The lubricant can effectively improve the surface glossiness of the composite material and reduce the friction coefficient of the material.
As a specific example, the second coupling agent may be a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent, and a chromium complex coupling agent. Preferably, the second coupling agent is a silane coupling agent. The second coupling agent can further improve the fluidity of the polyamide matrix, improve the brightness of the surface of the product, improve the compatibility of the organic matrix and the inorganic substance and improve the comprehensive mechanical property of the composite material.
The polyamide flame-retardant material is prepared by the following method: and mixing the polyamide, the flame retardant, the synergistic flame retardant, the heat-conducting filler, the glass fiber, the aluminum nitride compound, the lubricant and the second coupling agent, and then extruding and granulating.
As a specific example, the extrusion granulation process is carried out by adopting a double-screw extruder, wherein the temperature of a first zone of the double-screw extruder is 200-210 ℃, the temperature of a second zone of the double-screw extruder is 220-250 ℃, the temperature of a third zone of the double-screw extruder is 240-250 ℃, the temperature of a fourth zone of the double-screw extruder is 240-250 ℃, the temperature of a machine head of the double-screw extruder is 250-260 ℃, the total residence time is 1-2 min, and the pressure.
The invention provides a high-thermal-conductivity high-mechanical-property flame-retardant material, and provides a method for preparing an aluminum nitride compound from aluminum nitride, a polyolefin elastomer and other additives in advance to improve the compatibility of the aluminum nitride compound and a polyamide matrix aiming at the problems of reduction of the mechanical strength and unobvious improvement of the thermal conductivity coefficient of the material caused by adding more heat-conducting fillers. The amount of the heat conductive filler can be also reduced properly after the aluminum nitride compound is added. The prepared polyamide flame-retardant material has high heat conductivity coefficient and has the characteristics of high strength and high toughness.
The present invention is further described in detail with reference to specific examples and comparative examples, and the advantages of the technical solutions provided by the present invention will be apparent from the results of performance tests of the examples and comparative examples.
The raw materials selected in the following examples and comparative examples are all commercially available, and the specific types of some raw materials are only indicated for reference and do not represent any limitation on the specific sources of the raw materials.
The polyamide is selected from polycaprolactam;
the flame retardant is decabromodiphenylethane;
the synergistic flame retardant is sodium antimonate;
the heat-conducting filler is a compound product of aluminum oxide and magnesium oxide, and the specific model is Fushan Jinge PA-013;
the glass fiber is ground alkali-free glass fiber, and the specific model is EMG13-70C of megalithic corporation;
the lubricant is ethylene di-fatty acid amide, and the specific model is Karma TAF beneficial to the Netherlands;
the first and second coupling agents are both silane coupling agents, specifically Dow Corning KH-560.
The preparation of the aluminum nitride composite used in the following examples is as follows:
mixing aluminum nitride and a coupling agent, adding a polyolefin elastomer, maleic anhydride and dicumyl peroxide, banburying in an internal rubber mixing mill, and finally extruding and granulating by using a single-screw extruder.
The mixing was carried out in a high-speed mixer until homogeneous.
The temperature of the banburying process is 180 ℃, the rotating speed is 30 r/min-60 r/min, and the time is 5 min.
The following performance tests of the examples and comparative examples were carried out as follows:
the high-heat-conductivity polyamide flame-retardant granular material obtained by the preparation method is fully dried in a blast oven at 100 ℃ for 6 hours in advance, and then the dried granular material is subjected to injection molding sample preparation on an injection molding machine, wherein the temperature of the injection molding mold is controlled to be about 100 ℃.
The tensile strength test is carried out according to ISO 527-2 standard, the size of a test sample is 150 multiplied by 10 multiplied by 4mm, and the tensile speed is 50 mm/min; the bending performance test is carried out according to ISO 178 standard, the size of a test sample is 80 multiplied by 10 multiplied by 4mm, the bending speed is 2mm/min, and the span is 64 mm; the impact strength test of the simply supported beam is carried out according to ISO 179 standard, the size of a sample is 55 multiplied by 6 multiplied by 4mm, and the size of a gap is one third of the thickness of the sample; the flame retardant performance test is carried out according to UL94 standard; the thermal conductivity test was performed according to the steady state method of astm d5470 standard.
Wherein, the test results of tensile strength, elongation at break, bending strength, bending modulus and notch impact strength are used as the determination standard of comprehensive mechanical properties, and the flame retardant grade is used for determining the flame retardant property.
Example 1 and comparative examples 1 and 2 are used to reveal the role of aluminum nitride compound in a highly thermally conductive polyamide flame retardant material.
Example 1:
putting 43 parts of polycaprolactam, 50 parts of heat-conducting filler, 5 parts of aluminum nitride compound, 0.5 part of TAF and 0.4 part of KH-560 into a stirring barrel, and stirring for 15 minutes to fully mix the components. And then putting the uniformly mixed materials into a double-screw extruder, simultaneously adding 10 parts of ground alkali-free glass fiber from a side feeding port, and carrying out melting, mixing, extruding and granulating. In this example, the diameter of the screw of the twin-screw extruder was 58mm, the ratio of the length to the diameter of the screw was set at 36, and the extrusion temperature was 210 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 250 ℃ in the fourth zone, 260 ℃ in the head, the residence time was 2min, and the pressure was 15 MPa.
Comparative example 1:
43 parts of polycaprolactam, 8 parts of decabromodiphenylethane, 2.5 parts of sodium antimonate, 45 parts of heat-conducting filler and 0.5 part of TAF are placed into a stirring barrel and stirred for 15 minutes, so that the polycaprolactam, the decabromodiphenylethane, the sodium antimonate and the TAF are fully mixed. And then putting the uniformly mixed materials into a double-screw extruder for melting, mixing, extruding and granulating. In this example, the diameter of the screw of the twin-screw extruder was 36mm, the ratio of the length to the diameter of the screw was 36, and the extrusion temperature was 210 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 250 ℃ in the fourth zone, 260 ℃ in the head, the residence time was 2min, and the pressure was 15 MPa.
Comparative example 2:
43 parts of polycaprolactam, 45 parts of heat-conducting filler, 0.5 part of TAF and 0.5 min KH-560 are put into a stirring barrel and stirred for 15 minutes, so that the polycaprolactam and the heat-conducting filler are fully mixed. And then putting the uniformly mixed materials into a double-screw extruder for melting, mixing, extruding and granulating. In this example, the diameter of the screw of the twin-screw extruder was 36mm, the ratio of the length to the diameter of the screw was 36, and the extrusion temperature was 210 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 250 ℃ in the fourth zone, 260 ℃ in the head, the residence time was 2min, and the pressure was 15 MPa.
The results of the performance testing are shown in table 1 below:
TABLE 1
According to the data in table 1, it can be found that the elongation at break, the notched impact strength and the thermal conductivity of example 1 added with the aluminum nitride composite are significantly better than those of comparative examples 1 and 2, which shows that the aluminum nitride composite significantly improves the toughness and the thermal conductivity of the polyamide composite material, and proves that the "preparing the aluminum nitride composite by compounding the aluminum nitride and the polyolefin elastomer in advance effectively improves the compatibility of the composite material and the polyamide substrate, and is beneficial to the exertion of the thermal conductivity of the aluminum nitride and the improvement of the overall mechanical property of the material". The aluminum nitride compound plays an important role in solving the problems mentioned in the background art.
Example 2 and comparative examples 1, 3, 4 are used to verify that the introduction of the aluminum nitride compound can effectively reduce the amount of the heat-conducting filler while maintaining the thermal conductivity of the material.
Example 2:
62 parts of polycaprolactam, 10 parts of decabromodiphenylethane, 4 parts of sodium antimonate, 30 parts of heat-conducting filler, 10 parts of aluminum nitride compound, 0.5 part of TAF and 0.2 part of KH-560 are put into a stirring barrel and stirred for 15 minutes to be fully mixed. Then putting the uniformly mixed materials into a double-screw extruder, simultaneously adding 20 parts of ground alkali-free glass fiber from a side feeding port, and carrying out melting, mixing, extruding and granulating; in this example, the diameter of the screw of the twin-screw extruder was 35mm, the ratio of the length to the diameter of the screw was set at 36, and the extrusion temperature was 210 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 250 ℃ in the fourth zone, 260 ℃ in the head, the residence time was 2min, and the pressure was 13 MPa.
Comparative example 3:
putting 55 parts of polycaprolactam, 8 parts of decabromodiphenylethane, 3 parts of sodium antimonate, 38 parts of heat-conducting filler, 8 parts of aluminum nitride compound, 1 part of TAF and 0.3 part of KH-560 into a stirring barrel, and stirring for 15 minutes to fully mix the components. And then putting the uniformly mixed materials into a double-screw extruder, simultaneously adding 15 parts of ground alkali-free glass fiber from a side feeding port, and carrying out melting, mixing, extruding and granulating. In this example, the diameter of the screw of the twin-screw extruder was 50mm, the ratio of the length to the diameter of the screw was 42, and the extrusion temperature was 210 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 250 ℃ in the fourth zone, 260 ℃ in the head, the residence time was 2min, and the pressure was 16 MPa.
Comparative example 4:
putting 38 parts of polycaprolactam, 7 parts of decabromodiphenylethane, 2.5 parts of sodium antimonate, 50 parts of heat-conducting filler, 8 parts of aluminum nitride compound, 0.7 part of TAF and 0.5 part of KH-560 into a stirring barrel, and stirring for 15 minutes to fully mix the components. And then putting the uniformly mixed materials into a double-screw extruder, simultaneously adding 5 parts of ground alkali-free glass fiber from a side feeding port, and carrying out melting, mixing, extruding and granulating. In this example, the diameter of the screw of the twin-screw extruder was 65mm, the ratio of the length to the diameter of the screw was set to 32, and the extrusion temperature was 210 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 250 ℃ in the fourth zone, 260 ℃ in the head, the residence time was 2min, and the pressure was 14 MPa.
The results of the performance testing are shown in table 2 below:
TABLE 2
From the data in table 2, it can be seen that the polyamide material of comparative example 1 with 45 parts of heat conductive filler added has a significantly lower thermal conductivity than example 2 with 30 parts of heat conductive filler added, because 10 parts of aluminum nitride compound are added in example 2, indicating that the introduction of aluminum nitride compound can effectively reduce the amount of heat conductive filler. The heat conductivity coefficient of the polyamide material of comparative example 4 added with 50 parts of heat-conducting filler and 8 parts of aluminum nitride compound is only slightly higher than that of example 2 added with 30 parts of heat-conducting filler and 10 parts of aluminum nitride compound, which shows that the addition of the aluminum nitride compound greatly reduces the dosage of the heat-conducting filler under the condition of basically keeping the heat conductivity coefficient unchanged. The aluminum nitride compound reduces the dosage of the heat-conducting filler, avoids the problems of reduced mechanical property and unobvious increase of heat conductivity coefficient caused by adding excessive heat-conducting materials, and has very high practical value.
Based on the comparison of the performance test results in table 1 and table 2, it is clear that the aluminum nitride compound provided by the present invention has a significant effect on improving the thermal conductivity and toughness of the polyamide material. The aluminum nitride compound takes the polyolefin elastomer as a substrate, improves the compatibility between the aluminum nitride compound and the polyamide matrix, improves the toughness and the heat-conducting property, can also reduce the dosage of the heat-conducting filler, and avoids the defects caused by excessive addition of the heat-conducting filler. In addition, the aluminum nitride compound and the polyamide flame-retardant material raw material provided by the invention do not relate to a high-difficulty process or rare components, and have very high practical value.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (17)
1. The aluminum nitride compound is characterized by being prepared from the following raw material components in parts by weight:
2. the aluminum nitride composite according to claim 1, wherein the particle size of the aluminum nitride is 1 μm to 100 μm.
3. The aluminum nitride composite of claim 1, wherein the first coupling agent is selected from at least one of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent, and a chromium complex coupling agent.
4. A preparation method of an aluminum nitride compound is characterized by comprising the following steps:
the preparation method of the aluminum nitride compound according to any one of claims 1 to 3, wherein the aluminum nitride and the first coupling agent are mixed, and then the mixture is subjected to banburying, extrusion and granulation by adding the polyolefin elastomer, the maleic anhydride and the dicumyl peroxide.
5. The method for preparing the aluminum nitride compound according to claim 4, wherein the banburying temperature is 150 ℃ to 200 ℃, the rotation speed is 30r/min to 60r/min, and the time is 3min to 10 min.
6. The method for preparing the aluminum nitride compound as claimed in claim 4, wherein the extrusion granulation is performed by a single screw extruder, the extrusion temperature is 160 ℃ to 180 ℃, and the screw rotation speed is 70r/min to 150 r/min.
7. A flame retardant material comprising the aluminum nitride composite according to any one of claims 1 to 3.
8. The flame retardant material of claim 7, which is characterized by comprising the following raw material components in parts by weight:
9. flame retardant material according to claim 8, characterized in that the polyamide is selected from at least one of polycaprolactam and polyhexamethylene adipamide.
10. The flame retardant material of claim 8 wherein the polyamide has a viscosity coefficient of 2.0 to 4.5.
11. The flame retardant material of claim 8, wherein the flame retardant is a brominated flame retardant.
12. The flame retardant material of claim 8, wherein the synergistic flame retardant is an antimonide.
13. The flame retardant material of claim 8 wherein the thermally conductive filler is selected from at least one of magnesium oxide, aluminum oxide, magnesium hydroxide, aluminum hydroxide, magnesium nitride, aluminum nitride and boron nitride.
14. The flame retardant material of claim 8, wherein the glass fibers are milled glass fibers and have a length of 50 μm to 210 μm.
15. The flame retardant material of claim 8 wherein said lubricant is selected from at least one of silicone powder, ethylene bis stearamide and calcium stearate.
16. The preparation method of the flame retardant material is characterized by comprising the following steps of:
the flame-retardant material as claimed in any one of claims 8 to 15, wherein the raw material components are prepared according to the proportion, and the polyamide, the flame retardant, the synergistic flame retardant, the heat-conducting filler, the glass fiber, the aluminum nitride compound, the lubricant and the second coupling agent are mixed and then extruded for granulation.
17. The method for preparing the flame retardant material according to claim 16, wherein the extrusion granulation process is performed by using a twin-screw extruder, and the process of the twin-screw extruder is as follows: the temperature of the first area is 200-210 ℃, the temperature of the second area is 220-250 ℃, the temperature of the third area is 240-250 ℃, the temperature of the fourth area is 240-250 ℃, the temperature of the machine head is 250-260 ℃, the total retention time is 1-2 min, and the pressure is 12-18 MPa.
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