CN110591349A - Heat-conducting PA composite material and preparation method thereof - Google Patents
Heat-conducting PA composite material and preparation method thereof Download PDFInfo
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- CN110591349A CN110591349A CN201910995292.XA CN201910995292A CN110591349A CN 110591349 A CN110591349 A CN 110591349A CN 201910995292 A CN201910995292 A CN 201910995292A CN 110591349 A CN110591349 A CN 110591349A
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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Abstract
The invention discloses a heat-conducting PA composite material which is prepared from the following raw materials in percentage by weight: 625-45% of PA (polyamide), 2-6% of a toughening agent, 50-70% of a modified heat conducting agent, 0.1-0.5% of an antioxidant, 0.2-0.8% of a lubricant and 0.5-1.5% of a coupling agent, wherein the modified heat conducting agent is aluminum hydroxide subjected to surface treatment by a silane coupling agent; the invention also discloses a preparation method of the heat-conducting PA composite material; the heat-conducting PA composite material prepared by the invention has excellent heat conductivity, insulativity and mechanical property, and the application range of the PA material is expanded.
Description
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to a heat-conducting PA composite material and a preparation method thereof.
Background
The yield of nylon (PA) is at the beginning of engineering plastics, and the nylon (PA) has the advantages of excellent mechanical property, better wear resistance, excellent oil resistance and solvent resistance, corrosion resistance, self-lubrication, good processing performance and the like, so that the nylon (PA) is widely applied to related fields of electrical appliance industry, mechanical engineering, electrical engineering, automobile industry, aviation and the like at present, and especially the demand of LEDs is rapidly expanded. However, the thermal conductivity of nylon is generally 0.25W/(m.K), which limits its application in fields with heat dissipation and heat conduction requirements.
With the development of science and technology, heat-conducting plastics gradually enter people's lives and enter industrial production, the heat-conducting plastics are reasonable novel thermal interface materials, and the heat-conducting materials have excellent mechanical properties, such as light weight, strong chemical corrosion resistance, excellent electrical insulation performance, good dimensional stability, simple and convenient processing and forming, high heat conductivity coefficient and the like. For PA (nylon) materials, alumina is a commonly used inorganic heat-conducting agent, the heat conductivity coefficient of an alumina/PA composite material prepared from the alumina and the PA is improved along with the increase of the amount of the alumina, but the flowability, the processability and the impact resistance of the PA material can be reduced due to the excessively high amount of the alumina, and the commonly used inorganic heat-conducting agent has large surface polarity, poor dispersity in polymers, easy aggregation among filler particles and even separation from an organic phase at an interface, so that the circulation of heat between two-phase structures is blocked, and the heat conductivity is poor.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a thermally conductive PA composite material having excellent thermal conductivity, insulation properties and mechanical properties.
In order to achieve the purpose, the invention adopts the following technical scheme:
a heat-conducting PA composite material is composed of the following raw materials in percentage by weight: 625-45% of PA, 2-6% of toughening agent, 50-70% of modified heat conducting agent, 0.1-0.5% of antioxidant, 0.2-0.8% of lubricant and 0.5-1.5% of coupling agent.
Preferably, the material consists of the following raw materials in percentage by weight: PA 635%, toughening agent 3%, modified heat-conducting agent 60%, antioxidant 0.2%, lubricant 0.5% and coupling agent 1.3%.
Preferably, the material consists of the following raw materials in percentage by weight: PA 645%, toughening agent 3.5%, modified heat-conducting agent 50%, antioxidant 0.5%, lubricant 0.5%, and coupling agent 0.5%.
Preferably, the material consists of the following raw materials in percentage by weight: PA 625%, toughening agent 2.5%, modified heat-conducting agent 70%, antioxidant 0.2%, lubricant 0.8%, and coupling agent 1.5%.
Preferably, the toughening agent is KT-915 toughening agent; the antioxidant is 1098 antioxidant; the lubricant is ZnSt lubricant; the coupling agent is a silane coupling agent or a titanate coupling agent.
Preferably, the modified heat conducting agent is aluminum hydroxide subjected to surface treatment by a silane coupling agent, and the preparation method comprises the following steps: drying aluminum hydroxide at 90-100 deg.C for 30-60 min; silane coupling agent is added into the mixture according to the material-liquid ratio of 1: 40-60 g/g of the modified heat conducting agent is dissolved in ethanol, the pH value of the solution is adjusted to 3-4 by using acetic acid, then 30-50% of aluminum hydroxide of the total mass of the solution is added, the mixture is refluxed and stirred for 5-6h at the temperature of 60-80 ℃, and then stirred for 30-60min at room temperature, and the modified heat conducting agent is obtained after suction filtration, ethanol washing and drying.
Preferably, the silane coupling agent is one of KH-550, KH-560 or KH-570.
On the other hand, the invention also provides a preparation method of the heat-conducting PA composite material, which comprises the following steps:
s1, drying the PA6 and the modified heat-conducting agent at 90-105 ℃ for 2-4h, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
and S2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating to obtain the heat-conducting PA composite material.
Preferably, the heating temperature of the twin-screw extruder in S2 is 200-. The heating temperature of the double-screw extruder is selected according to the properties of various raw materials, the heating temperature is preferred by the inventor according to the physical properties of the components of the raw materials, in the temperature range, the various raw materials can be melted thoroughly and mixed and melted fully, the incomplete melting and mixing caused by the low temperature is avoided, the cracking and the deterioration caused by the high temperature are avoided, and the raw materials can be mixed, melted and combined fully to obtain the high-quality performance sought by the invention.
Compared with the prior art, the invention has the beneficial technical effects that:
the heat-conducting PA composite material disclosed by the invention has the advantages that the silane coupling agent is used for carrying out surface treatment modification on aluminum hydroxide, so that the interaction force between the aluminum hydroxide and PA6 can be increased, and the phonon scattering at the interface is reduced, so that the interface thermal resistance is reduced, in addition, the modified aluminum hydroxide has a better dispersion effect in PA6, is not easy to agglomerate and deposit, can form a more complete heat-conducting net or chain structure, and the heat-conducting property is obviously improved.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A heat-conducting PA composite material is composed of the following raw materials in percentage by weight: PA 635%, KT-915 toughening agent 3%, modified heat-conducting agent 60%, 1098 antioxidant 0.2%, ZnSt lubricant 0.5% and silane coupling agent 1.3%;
the modified heat-conducting agent is aluminum hydroxide subjected to surface treatment by a silane coupling agent KH-560, and the preparation method comprises the following steps: drying aluminum hydroxide at 100 deg.C for 60 min; mixing a silane coupling agent KH-560 according to a material-liquid ratio of 1: dissolving 50 g/g in ethanol, adjusting the pH value of the solution to 3.5 by using acetic acid, then adding aluminum hydroxide accounting for 40% of the total mass of the solution, refluxing at 70 ℃, stirring for 5.5h, stirring at room temperature for 45min, and obtaining the modified heat-conducting agent after suction filtration, ethanol washing and drying.
A preparation method of a heat-conducting PA composite material comprises the following steps:
s1, drying the PA6 and the modified heat-conducting agent at 100 ℃ for 3 hours, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
s2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating, wherein the heating temperature of the double-screw extruder is 200 ℃ in the first zone, 220 ℃ in the second zone, 230 ℃ in the third zone, 230 ℃ in the fourth zone, 230 ℃ in the fifth zone, 230 ℃ in the sixth zone, 225 ℃ in the seventh zone, 225 ℃ in the eighth zone and 225 ℃ in the ninth zone, so that the heat-conducting PA composite material is obtained.
Example 2
A heat-conducting PA composite material is composed of the following raw materials in percentage by weight: PA 645%, KT-915 toughening agent 3.5%, modified heat conducting agent 50%, 1098 antioxidant 0.5%, ZnSt lubricant 0.5%, titanate coupling agent 0.5%;
the modified heat-conducting agent is aluminum hydroxide subjected to surface treatment by using a silane coupling agent KH-550, and the preparation method comprises the following steps: drying aluminum hydroxide at 90 deg.C for 30 min; silane coupling agent is added into the mixture according to the material-liquid ratio of 1: 40 g/g of the modified heat conducting agent is dissolved in ethanol, the pH value of the solution is adjusted to 3 by using acetic acid, then aluminum hydroxide accounting for 30 percent of the total mass of the solution is added, the mixture is refluxed and stirred for 6 hours at the temperature of 60 ℃, then stirred for 30 minutes at room temperature, and the modified heat conducting agent is obtained after suction filtration, ethanol washing and drying.
A preparation method of a heat-conducting PA composite material comprises the following steps:
s1, drying the PA6 and the modified heat-conducting agent at 90 ℃ for 4 hours, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
s2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating, wherein the heating temperature of the double-screw extruder is 210 ℃ in the first zone, 225 ℃ in the second zone, 235 ℃ in the third zone, 235 ℃ in the fourth zone, 235 ℃ in the fifth zone, 235 ℃ in the sixth zone, 230 ℃ in the seventh zone, 230 ℃ in the eighth zone and 230 ℃ in the ninth zone, so as to obtain the heat-conducting PA composite material.
Example 3
A heat-conducting PA composite material is composed of the following raw materials in percentage by weight: PA 625%, KT-915 toughening agent 2.5%, modified heat conducting agent 70%, 1098 antioxidant 0.2%, ZnSt lubricant 0.8% and silane coupling agent 1.5%;
the modified heat conducting agent is aluminum hydroxide subjected to surface treatment by a silane coupling agent KH-570, and the preparation method comprises the following steps: drying aluminum hydroxide at 95 ℃ for 60min for later use; silane coupling agent is added into the mixture according to the material-liquid ratio of 1: 60 g/g of the modified heat conducting agent is dissolved in ethanol, the pH value of the solution is adjusted to 4 by using acetic acid, then aluminum hydroxide with the total mass of 50% of the solution is added, the mixture is refluxed and stirred for 5 hours at the temperature of 80 ℃, and then stirred for 60 minutes at room temperature, and the modified heat conducting agent is obtained after the processes of suction filtration, ethanol washing and drying.
A preparation method of a heat-conducting PA composite material comprises the following steps:
s1, drying the PA6 and the modified heat-conducting agent at 105 ℃ for 2 hours, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
s2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating, wherein the heating temperature of the double-screw extruder is 220 ℃ in the first zone, 230 ℃ in the second zone, 235 ℃ in the third zone, 235 ℃ in the fourth zone, 235 ℃ in the fifth zone, 235 ℃ in the sixth zone, 225 ℃ in the seventh zone, 225 ℃ in the eighth zone and 225 ℃ in the ninth zone, so that the heat-conducting PA composite material is obtained.
Comparative example 1
The difference from example 1 is that the aluminum hydroxide heat conductive agent is not subjected to surface treatment.
A heat-conducting PA composite material is composed of the following raw materials in percentage by weight: PA 635%, KT-915 toughening agent 3%, aluminum hydroxide heat conducting agent 60%, 1098 antioxidant 0.2%, ZnSt lubricant 0.5% and silane coupling agent 1.3%;
a preparation method of a heat-conducting PA composite material comprises the following steps:
s1, drying the PA6 and the heat conducting agent at 100 ℃ for 3 hours, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
s2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating, wherein the heating temperature of the double-screw extruder is 200 ℃ in the first zone, 220 ℃ in the second zone, 230 ℃ in the third zone, 230 ℃ in the fourth zone, 230 ℃ in the fifth zone, 230 ℃ in the sixth zone, 225 ℃ in the seventh zone, 225 ℃ in the eighth zone and 225 ℃ in the ninth zone, so that the heat-conducting PA composite material is obtained.
Comparative example 2
The difference from the example 1 is that the proportion of the PA6 and the modified heat-conducting agent is changed, and the content of the modified heat-conducting agent is higher.
A heat-conducting PA composite material is composed of the following raw materials in percentage by weight: PA 615%, KT-915 toughening agent 3%, modified heat-conducting agent 80%, 1098 antioxidant 0.2%, ZnSt lubricant 0.5%, and silane coupling agent 1.3%;
the modified heat-conducting agent is aluminum hydroxide subjected to surface treatment by a silane coupling agent KH-560, and the preparation method comprises the following steps: drying aluminum hydroxide at 100 deg.C for 60 min; mixing a silane coupling agent KH-560 according to a material-liquid ratio of 1: dissolving 50 g/g in ethanol, adjusting the pH value of the solution to 3.5 by using acetic acid, then adding aluminum hydroxide accounting for 40% of the total mass of the solution, refluxing at 70 ℃, stirring for 5.5h, stirring at room temperature for 45min, and obtaining the modified heat-conducting agent after suction filtration, ethanol washing and drying.
A preparation method of a heat-conducting PA composite material comprises the following steps:
s1, drying the PA6 and the modified heat-conducting agent at 100 ℃ for 3 hours, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
s2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating, wherein the heating temperature of the double-screw extruder is 200 ℃ in the first zone, 220 ℃ in the second zone, 230 ℃ in the third zone, 230 ℃ in the fourth zone, 230 ℃ in the fifth zone, 230 ℃ in the sixth zone, 225 ℃ in the seventh zone, 225 ℃ in the eighth zone and 225 ℃ in the ninth zone, so that the heat-conducting PA composite material is obtained.
Comparative example 3
The difference from the example 1 is that the proportion of the PA6 and the modified heat-conducting agent is changed, and the content of the modified heat-conducting agent is lower.
A heat-conducting PA composite material is composed of the following raw materials in percentage by weight: PA 655 percent, KT-915 toughening agent 3 percent, modified heat conducting agent 40 percent, 1098 antioxidant 0.2 percent, ZnSt lubricant 0.5 percent and silane coupling agent 1.3 percent;
the modified heat-conducting agent is aluminum hydroxide subjected to surface treatment by a silane coupling agent KH-560, and the preparation method comprises the following steps: drying aluminum hydroxide at 100 deg.C for 60 min; mixing a silane coupling agent KH-560 according to a material-liquid ratio of 1: dissolving 50 g/g in ethanol, adjusting the pH value of the solution to 3.5 by using acetic acid, then adding aluminum hydroxide accounting for 40% of the total mass of the solution, refluxing at 70 ℃, stirring for 5.5h, stirring at room temperature for 45min, and obtaining the modified heat-conducting agent after suction filtration, ethanol washing and drying.
A preparation method of a heat-conducting PA composite material comprises the following steps:
s1, drying the PA6 and the modified heat-conducting agent at 100 ℃ for 3 hours, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
s2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating, wherein the heating temperature of the double-screw extruder is 200 ℃ in the first zone, 220 ℃ in the second zone, 230 ℃ in the third zone, 230 ℃ in the fourth zone, 230 ℃ in the fifth zone, 230 ℃ in the sixth zone, 225 ℃ in the seventh zone, 225 ℃ in the eighth zone and 225 ℃ in the ninth zone, so that the heat-conducting PA composite material is obtained.
Performance testing and evaluation
The thermally conductive PA composites prepared in examples 1-3 and comparative examples 1-3 were subjected to performance testing, and the test results are detailed in table 1 below.
TABLE 1
As can be seen from Table 1, the heat-conducting PA materials prepared in the embodiments 1-3 of the invention have excellent thermal properties and mechanical properties; comparative example 1 the thermal and mechanical properties were poor because the heat conducting agent was not surface treated; comparative example 2 the mechanical properties were rather impaired due to the excessively high addition of the modified thermal conductor; comparative example 3 because the addition amount of the modified heat-conducting agent is too low, the thermal property and the mechanical property are poor, which shows that the heat-conducting agent is subjected to surface treatment modification, and the proportion of each raw material component is optimized, so that the prepared product has excellent thermal property and mechanical property, wherein the proportion of each raw material in the embodiment 1 is most reasonable.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (9)
1. The heat-conducting PA composite material is characterized by comprising the following raw materials in percentage by weight: 625-45% of PA, 2-6% of toughening agent, 50-70% of modified heat conducting agent, 0.1-0.5% of antioxidant, 0.2-0.8% of lubricant and 0.5-1.5% of coupling agent.
2. The heat-conducting PA composite material as claimed in claim 1, which is prepared from the following raw materials in percentage by weight: PA 635%, toughening agent 3%, modified heat-conducting agent 60%, antioxidant 0.2%, lubricant 0.5% and coupling agent 1.3%.
3. The heat-conducting PA composite material as claimed in claim 1, which is prepared from the following raw materials in percentage by weight: PA 645%, toughening agent 3.5%, modified heat-conducting agent 50%, antioxidant 0.5%, lubricant 0.5%, and coupling agent 0.5%.
4. The heat-conducting PA composite material as claimed in claim 1, which is prepared from the following raw materials in percentage by weight: PA 625%, toughening agent 2.5%, modified heat-conducting agent 70%, antioxidant 0.2%, lubricant 0.8%, and coupling agent 1.5%.
5. The thermally conductive PA composite of any of claims 1-4, wherein the toughening agent is a KT-915 toughening agent; the antioxidant is 1098 antioxidant; the lubricant is ZnSt lubricant; the coupling agent is a silane coupling agent or a titanate coupling agent.
6. The thermally conductive PA composite material according to any one of claims 1 to 4, wherein the modified thermally conductive agent is aluminum hydroxide surface-treated with a silane coupling agent, and the preparation method comprises the following steps: drying aluminum hydroxide at 90-100 deg.C for 30-60 min; silane coupling agent is added into the mixture according to the material-liquid ratio of 1: 40-60 g/g of the modified heat conducting agent is dissolved in ethanol, the pH value of the solution is adjusted to 3-4 by using acetic acid, then 30-50% of aluminum hydroxide of the total mass of the solution is added, the mixture is refluxed and stirred for 5-6h at the temperature of 60-80 ℃, and then stirred for 30-60min at room temperature, and the modified heat conducting agent is obtained after suction filtration, ethanol washing and drying.
7. The thermally conductive PA composite of claim 6, wherein the silane coupling agent is one of KH-550, KH-560, or KH-570.
8. A method of making a thermally conductive PA composite according to any of claims 1 to 7, comprising the steps of:
s1, drying the PA6 and the modified heat-conducting agent at 90-105 ℃ for 2-4h, mixing with the toughening agent, the antioxidant, the lubricant and the coupling agent, adding into a stirrer, and uniformly mixing to obtain a mixture;
and S2, putting the mixture into a hopper of a double-screw extruder, and extruding and granulating to obtain the heat-conducting PA composite material.
9. The preparation method as claimed in claim 8, wherein the heating temperature of the twin-screw extruder in S2 is one zone of 200-.
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Application publication date: 20191220 |