CN110885554A - Nylon 66 composite material and preparation method and application thereof - Google Patents
Nylon 66 composite material and preparation method and application 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a nylon 66 composite material and a preparation method and application thereof, belonging to the technical field of composite materials. According to the mass percentage, the nylon 66 composite material provided by the invention comprises the following preparation raw materials: 45.4-90.8% of nylon 66; 5-45.4% of linear nylon 6; 3-8% of a toughening agent, wherein the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylate double functionalization; 0.1-2% of a lubricant; 0.1-2% of nucleating agent; 0.1-2% of antioxidant. According to the invention, nylon 66 and linear nylon 6 are compounded, and a toughening agent, a lubricant, a nucleating agent and an antioxidant are added, so that the obtained nylon 66 composite material has excellent comprehensive performance and is suitable for preparing automobile fasteners. Meanwhile, the linear nylon 6 as the matrix material has lower cost than nylon 66, and the relative production cost is obviously reduced after the linear nylon 6 is compounded.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a nylon 66 composite material and a preparation method and application thereof.
Background
Nylon 66 is polyhexamethylene adipamide, abbreviated as PA66 resin, is one of five engineering plastics in the world, and is widely applied to the fields of automobiles, household appliances, electronic and electric appliances and the like due to high fatigue strength and rigidity, good heat resistance, low friction coefficient and good wear resistance. With the acceleration of the light weight process of automobiles, the application of PA66 in the field of automobiles is wider and more demanding, and in order to meet the requirements of markets on material flowability, rapid injection molding and the like, modification research on PA66 resin is needed.
In the pure PA66 resin modified material, the problems of high molding shrinkage rate (1.6-1.9%), poor rebound resilience, low crystallization efficiency, poor fluidity, unstable workpiece size, high raw material cost and the like exist. At present, a compound material of PA66 resin and PA6 resin (namely nylon 6) is modified, for example, in a patent CN 201611014288.3, nylon 66 and branched nylon 6 are compounded, maleic anhydride grafted POE is used as a toughening agent, and a lubricant, an antioxidant and the like are added to prepare the toughened nylon 66 material, but the mechanical property, the insertion and extraction force performance and the crystallization effect of the material are still to be improved, so that the material is not suitable for being used under special working conditions, such as preparing an automobile buckle.
Disclosure of Invention
The invention aims to provide a nylon 66 composite material, and a preparation method and application thereof, and the nylon 66 composite material provided by the invention has low molding shrinkage rate, high crystallization efficiency, high fluidity and high resilience, and can meet the requirements of an automobile buckle on the insertion and extraction force.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a nylon 66 composite material which comprises the following preparation raw materials in percentage by mass:
45.4-90.8% of nylon 66;
5-45.4% of linear nylon 6;
3-8% of a toughening agent, wherein the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylate double functionalization;
0.1-2% of a lubricant;
0.1-2% of nucleating agent;
0.1-2% of antioxidant.
Preferably, the relative viscosity of the nylon 66 is 2.4-2.7.
Preferably, the relative viscosity of the linear nylon 6 is 2.4-2.9.
Preferably, the total grafting ratio of the maleic anhydride and the acrylic ester in the toughening agent is 0.8-1.3%.
Preferably, the lubricant is a mixture of ultra-high molecular weight silicone and calcium stearate, wherein the mass ratio of the ultra-high molecular weight silicone to the calcium stearate is 4: 1; the ultra-high molecular weight organic silicon takes low-density polyethylene as a matrix.
Preferably, the nucleating agent is an organic salt nucleating agent.
Preferably, the antioxidant is a mixture of an antioxidant 1098 and an antioxidant 168, wherein the mass ratio of the antioxidant 1098 to the antioxidant 168 is 1: 2.
the invention provides a preparation method of the nylon 66 composite material in the technical scheme, which comprises the following steps:
mixing nylon 66, linear nylon 6, a toughening agent, a lubricant, a nucleating agent and an antioxidant, and then carrying out plasticizing melting, extrusion and granulation to obtain the nylon 66 composite material.
Preferably, the plasticizing melting and extruding are carried out in a double-screw extruder, and the rotating speed of a screw is 200-350 rpm;
the machine barrel of the double-screw extruder is divided into 11 sections of temperature control areas from the blanking end to the machine head, and the temperature of each section of temperature control area is 265 ℃, 270 ℃, 265 ℃, 260 ℃, 265 ℃ and 270 ℃ in sequence.
The invention provides an application of the nylon 66 composite material in the technical scheme or the nylon 66 composite material prepared by the preparation method in the technical scheme in preparation of an automobile buckle.
The invention provides a nylon 66 composite material which comprises the following preparation raw materials in percentage by mass: 45.4-90.8% of nylon 66; 5-45.4% of linear nylon 6; 3-8% of a toughening agent, wherein the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylate double functionalization; 0.1-2% of a lubricant; 0.1-2% of nucleating agent; 0.1-2% of antioxidant. According to the invention, nylon 66 and linear nylon 6 are compounded, and a toughening agent, a lubricant, a nucleating agent and an antioxidant are added, so that the obtained nylon 66 composite material has excellent comprehensive performance and is suitable for preparing automobile fasteners. Specifically, compared with branched nylon 6, the linear nylon 6 is added to be compounded with nylon 66, so that the crystallization effect of the material is improved; the addition of the POE with maleic anhydride and acrylic ester dual-functionalization as the toughening agent is beneficial to improving the toughness and low-temperature resistance of the material and ensuring the requirements of the material on mechanical properties such as insertion and extraction force, impact and the like; the lubricant is added, so that the surface friction coefficient of the material is favorably reduced, the surface smoothness effect of the material is improved while other excellent properties of the material are maintained, the material has higher fluidity and demolding property, and the complex workpiece, namely the automobile buckle, is easy to machine and form; the addition of the nucleating agent is beneficial to improving the mechanical properties of the material such as stretching, bending and impact, improving the crystallization efficiency, the crystal granularity and the crystallization integrity of the material, shortening the molding period, improving the dimensional stability of the material and improving the demolding effect of the material to a certain extent. The toughening agent, the lubricant and the nucleating agent are matched for use, so that the flowability, the crystallization efficiency and the mechanical property of the material are improved, the risk of size fluctuation possibly caused by poor dispersibility, poor crystallization capacity and the like is reduced, the homogenization and the easy processing property of the material in the injection molding process are improved, and the production cost is effectively reduced. Therefore, the nylon 66 composite material provided by the invention has lower molding shrinkage, higher crystallization efficiency, fluidity and resilience, and can meet the requirements of automobile buckles on the insertion and extraction force; in the aspect of processing and forming of the automobile buckle, the demoulding of a workpiece is facilitated, the stability of the size of the workpiece is ensured, the processing and forming effect on the workpiece with a thin wall or a long flow is remarkable, the reject ratio of the workpiece is effectively reduced, and the production efficiency is improved; meanwhile, the linear nylon 6 as the matrix material has lower cost than nylon 66, and the relative production cost is obviously reduced after the linear nylon 6 is compounded.
Detailed Description
The invention provides a nylon 66 composite material which comprises the following preparation raw materials in percentage by mass:
45.4-90.8% of nylon 66;
5-45.4% of linear nylon 6;
3-8% of a toughening agent, wherein the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylate double functionalization;
0.1-2% of a lubricant;
0.1-2% of nucleating agent;
0.1-2% of antioxidant.
The preparation raw materials of the nylon 66 composite material comprise, by mass, 45.4-90.8% of nylon 66, preferably 45.4-75%, and more preferably 45.4-65%. The relative viscosity of the nylon 66 (or called PA66 resin) is preferably 2.4-2.7. In an embodiment of the invention, the PA66 resin was purchased from engineering plastics, llc, of flat top mountain mare, model number EPR 27.
The raw materials for preparing the nylon 66 composite material comprise, by mass, 5-45.4% of linear nylon 6, preferably 15-45.4%, and more preferably 25-45.4%. The relative viscosity of the linear nylon 6 (or called linear PA6 resin) is preferably 2.4-2.9. In an embodiment of the present invention, the linear PA6 resin was purchased from yueyang chemical corporation, han, a specific model number YH 800. Compared with branched nylon 6, the invention adds linear nylon 6 to be compounded with nylon 66, which is beneficial to improving the crystallization effect of the material.
According to the invention, the preparation raw materials of the nylon 66 composite material comprise 3-8% of toughening agent by mass percentage, preferably 5-8%, more preferably 6-8%; the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylic ester difunctional, and the total grafting rate of the maleic anhydride and the acrylic ester in the toughening agent is preferably 0.8-1.3%. In an embodiment of the present invention, the toughening agent is purchased from Shenyang Ketong plastics Co., Ltd, with a specific model number of KT-915. The invention adopts the maleic anhydride and acrylic ester difunctional POE as the toughening agent, is beneficial to improving the toughness and low temperature resistance of the material, ensures the requirements of the material on the mechanical properties such as insertion and extraction force, impact and the like, has better toughening property compared with the maleic anhydride grafted POE, and ensures that the obtained nylon 66 composite material has higher impact resistance advantage.
The preparation raw materials of the nylon 66 composite material comprise 0.1-2% of lubricant by mass percentage, and preferably 0.3-1.5%. In the present invention, the lubricant is preferably a mixture of ultra-high molecular weight silicone and calcium stearate, wherein the mass ratio of the ultra-high molecular weight silicone to the calcium stearate is preferably 4: 1; the ultra-high molecular weight silicone is preferably based on Low Density Polyethylene (LDPE). In an embodiment of the present invention, the ultra-high molecular weight silicone is purchased from Beijing Huayutong Rui, with the specific model being GT-002. The invention takes the mixture of the ultra-high molecular weight organic silicon and the calcium stearate as the lubricant, wherein the ultra-high molecular weight organic silicon can effectively improve the lubricity of the system, is beneficial to demoulding and improving the fluidity of the material, and the calcium stearate is both a demoulding agent and a lubricant, is beneficial to the demoulding effect of the material.
The preparation raw materials of the nylon 66 composite material comprise 0.1-2% of nucleating agent by mass percentage, preferably 0.2-1.5%, and more preferably 0.3-0.6%. In the invention, the nucleating agent is preferably an organic salt nucleating agent, and specifically can be a product with the model number of SN-02PA purchased from Beijing Huayutong Rui or a product with the model number of P22 purchased from Bruggeman; in the embodiment of the invention, the organic salt nucleating agent is a product with model number SN-02PA purchased from Beijing Huayu Toni. The invention utilizes the nucleating agent to improve the mechanical properties of the material such as stretching, bending and impact, improves the crystallization efficiency, the crystal granularity and the crystallization integrity of the material, shortens the molding period, improves the dimensional stability of the material and simultaneously improves the demolding effect of the material to a certain extent. And the nucleating agent is matched with the toughening agent and the lubricant for use, so that the fluidity, the crystallization efficiency and the mechanical property of the material are improved, the risk of size fluctuation possibly caused by poor dispersibility, poor crystallization capacity and the like is reduced, the homogenization and the easy processing property of the material in the injection molding process are improved, and the production cost is effectively reduced.
The preparation raw materials of the nylon 66 composite material comprise 0.1-2% of antioxidant, preferably 0.2-1.5%, and more preferably 0.3-0.6% by mass. In the invention, the antioxidant is preferably a mixture of an antioxidant 1098 and an antioxidant 168, wherein the mass ratio of the antioxidant 1098 to the antioxidant 168 is preferably 1: 2. according to the invention, the antioxidant is utilized to improve the anti-aging performance of the material, so that the obtained nylon 66 composite material has the advantages of anti-aging and prolonged service life.
The invention provides a preparation method of a nylon 66 composite material, which comprises the following steps:
mixing nylon 66, linear nylon 6, a toughening agent, a lubricant, a nucleating agent and an antioxidant, and then carrying out plasticizing melting, extrusion and granulation to obtain the nylon 66 composite material.
The invention mixes nylon 66, linear nylon 6, toughening agent, lubricant, nucleating agent and antioxidant to obtain a mixed material. The invention has no special limitation on the mixing, and can be obtained by uniformly mixing all the preparation raw materials; specifically, each raw material may be placed in a mixer and mixed for 15min at a speed of 10 rpm.
After the mixed material is obtained, the mixed material is subjected to plasticizing melting, extrusion and grain cutting to obtain the nylon 66 composite material. In the invention, the plasticizing melting and extrusion are preferably carried out in a double-screw extruder, and the screw rotating speed is preferably 200-350 rpm; the machine barrel of the double-screw extruder is divided into 11 sections of temperature control areas from the blanking end to the machine head, the temperature of each section of temperature control area is preferably 265 ℃, 270 ℃, 265 ℃, 260 ℃, 265 ℃ and 270 ℃ in sequence, and under the condition, the temperature of plasticizing and melting can be controlled to be 265 +/-5 ℃, so that the plasticizing and melting can be smoothly carried out, and the obtained nylon 66 composite material has better performance.
In the present invention, it is preferable that the extruding step further includes cooling the extruded material before the dicing step, and the dicing step further includes packaging the material obtained after the dicing step to obtain the nylon 66 composite material. The present invention is not particularly limited with respect to the cooling, pelletizing and packaging, and may be carried out in a manner conventional in the art.
The invention provides an application of the nylon 66 composite material in the technical scheme or the nylon 66 composite material prepared by the preparation method in the technical scheme in preparation of an automobile buckle.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples were prepared using the following starting materials:
the PA66 resin has the relative viscosity of 2.4-2.7, is purchased from Hippocampus engineering plastics Limited liability company, and has the specific model of EPR 27;
the linear PA6 resin has the relative viscosity of 2.4-2.9, and is purchased from Yueyang chemical industries, Inc. in Hunan, and the specific model is YH 800;
the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylate dual-functional groups, which is purchased from Shenyang Ketong plastics Co., Ltd, and has the specific model of KT-915;
the nucleating agent is organic salt nucleating agent purchased from Beijing Huayutong Rui, and its specific model is SN-02 PA;
the antioxidant is a mixture of an antioxidant 1098 and an antioxidant 168, wherein the mass ratio of the antioxidant 1098 to the antioxidant 168 is 1: 2;
the lubricant is a mixture of ultrahigh molecular weight organosilicon and calcium stearate, wherein the mass ratio of the ultrahigh molecular weight organosilicon to the calcium stearate is 4: 1; the ultra-high molecular weight organosilicon takes Low Density Polyethylene (LDPE) as a matrix, is purchased from Beijing Huayutong Rui, and has a specific model of GT-002.
Example 1
A preparation method of a nylon 66 composite material comprises the following steps:
① ingredients including 70kg of PA66 resin, 30kg of linear PA6 resin, 8kg of toughening agent, 0.5kg of lubricant, 0.5kg of nucleating agent and 0.5kg of antioxidant.
② mixing materials, pouring the prepared raw materials into a mixer, mixing at 10rpm for 15min to obtain a mixture, and storing at room temperature.
③, plasticizing and melting the mixture by a double-screw extruder, extruding, cooling, cutting into granules and packaging to obtain the nylon 66 composite material, wherein the rotation speed of the screw is 350rpm, the machine barrel of the double-screw extruder is divided into 11 sections of temperature control areas from the blanking end to the machine head, and the temperature of each section of temperature control area is 265 ℃, 270 ℃, 265 ℃, 260 ℃, 265 ℃ and 270 ℃ in sequence.
Example 2
The preparation method of the nylon 66 composite material in the embodiment is basically the same as that in the embodiment 1, except that the preparation raw materials comprise the following components:
60kg of PA66 resin, 40kg of linear PA6 resin, 8kg of toughening agent, 1kg of lubricant, 0.5kg of nucleating agent and 0.5kg of antioxidant.
Example 3
The preparation method of the nylon 66 composite material in the embodiment is basically the same as that in the embodiment 1, except that the preparation raw materials comprise the following components:
50kg of PA66 resin, 50kg of linear PA6 resin, 8kg of toughening agent, 1.5kg of lubricant, 0.5kg of nucleating agent and 0.5kg of antioxidant.
Comparative example
The preparation method of the nylon 66 composite material in this example is substantially the same as that of example 3, except that the toughening agent is omitted from the raw materials for preparation.
The performance of the nylon 66 composite materials prepared in examples 1-3 and comparative example was tested as follows:
the tensile strength is detected according to the GBT 1040.1-2006 standard;
the bending strength is detected according to the GB-T9341-2008 standard;
the notch impact strength is detected according to the GBT 1043.1-2008 standard;
the non-notch impact strength is detected according to the GBT 1043.1-2008 standard;
the molding shrinkage is detected according to the GBT 17037.4-2003 standard;
the melt flow rate is detected according to the GBT-3682-;
the density was measured according to GBT 1033.1-2008.
The normal-temperature insertion and extraction force test is as follows:
1) testing device
a. A tensile testing machine: the device is provided with an automatic recording device and an automatic centering clamp, and the error of the force value indication is less than 1%;
b. sample piece: HC-CF01 buckle;
c. tooling: the tool meets the requirements of HC-CF01 buckle, the long round hole is 7mm multiplied by 12mm, and the sheet metal thickness is 1.2 mm;
2) test conditions
a. Standard state: the temperature is 23 +/-2 ℃, the relative humidity is 50 +/-5%, and the test sample is kept in the test environment for at least 1h before testing;
b. the moving speed of the clamp of the tensile testing machine is 50 mm/min;
3) test procedure
a. Installing an HC-CF01 buckle sample piece on a clamp of a tensile testing machine;
b. after aligning the tooling hole and the central line of the buckle, testing the insertion and extraction force;
4) test results
And taking the average value of five tests as a final result, and accurately obtaining two digits after decimal point.
The high-temperature-resistant insertion and extraction force test is as follows:
five HC-CF01 buckle samples were placed in a 210 ℃ oven and baked for 30min, cooled to room temperature, and tested according to the normal temperature insertion and extraction force test described above.
The results are shown in Table 1.
TABLE 1 Performance test results for Nylon 66 composites prepared in examples 1-3 and comparative examples
| Test items | Unit of | Example 1 | Example 2 | Example 3 | Comparative example | Standard fastener |
| Tensile strength | MPa | 59.4 | 58.2 | 57.5 | 68.7 | ≥50 |
| Bending strength | MPa | 79.5 | 78.2 | 77.0 | 96.9 | ≥70 |
| Notched impact strength | kJ/m2 | 18.8 | 19.5 | 20.0 | 6.3 | ≥17 |
| Non-notched impact strength | kJ/m2 | NB | NB | NB | NB | NB |
| Molding shrinkage ratio | ％ | 1.25～1.31 | 1.38～1.43 | 1.29～1.36 | 1.85～1.95 | 1.2～1.7 |
| Melt flow rate | g/10min | 22.2 | 25.1 | 28.4 | 31.0 | 20～30 |
| Density of | g/cm3 | 1.16 | 1.14 | 1.12 | 1.18 | ≤1.16 |
| Insertion force at normal temperature | N | 49.34 | 45.87 | 42.76 | Brittle fracture | ≤60 |
| Normal temperature drawing force | N | 192.38 | 170.17 | 156.65 | Brittle fracture | ≥150 |
| High temperature insertion force resistance | \ | Without brittle fracture | Without brittle fracture | Without brittle fracture | Brittle fracture | Without brittle fracture |
| High temperature resistant withdrawal force | \ | Without brittle fracture | Without brittle fracture | Without brittle fracture | Brittle fracture | Without brittle fracture |
Note: in table 1 "NB" stands for out of measurement range, i.e. the material is continuously within the measurement range.
As can be seen from table 1, in comparison with the comparative examples in examples 1 to 3, by using different compounding ratios of PA66 and linear PA6 and adding a toughening agent, the notch impact strength and the insertion and extraction force performance of the nylon 66 composite material prepared by the invention are significantly enhanced, and the molding shrinkage and the melt flow rate are significantly reduced; compared with the snap standard, the nylon 66 composite material in the embodiments 1-3 has various performances meeting the requirements of the snap standard.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The nylon 66 composite material is characterized by comprising the following preparation raw materials in percentage by mass:
45.4-90.8% of nylon 66;
5-45.4% of linear nylon 6;
3-8% of a toughening agent, wherein the toughening agent is POE (polyolefin elastomer) with maleic anhydride and acrylate double functionalization;
0.1-2% of a lubricant;
0.1-2% of nucleating agent;
0.1-2% of antioxidant.
2. The nylon 66 composite material of claim 1, wherein the nylon 66 has a relative viscosity of 2.4-2.7.
3. The nylon 66 composite of claim 1, wherein the linear nylon 6 has a relative viscosity of 2.4 to 2.9.
4. The nylon 66 composite material of claim 1, wherein the total grafting ratio of the maleic anhydride and the acrylic ester in the toughening agent is 0.8-1.3%.
5. The nylon 66 composite of claim 1, wherein the lubricant is a mixture of ultra-high molecular weight silicone and calcium stearate, wherein the mass ratio of ultra-high molecular weight silicone to calcium stearate is 4: 1; the ultra-high molecular weight organic silicon takes low-density polyethylene as a matrix.
6. The nylon 66 composite material of claim 1, wherein the nucleating agent is an organic salt nucleating agent.
7. The nylon 66 composite material as claimed in claim 1, wherein the antioxidant is a mixture of an antioxidant 1098 and an antioxidant 168, wherein the mass ratio of the antioxidant 1098 to the antioxidant 168 is 1: 2.
8. a method for preparing the nylon 66 composite material as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps:
mixing nylon 66, linear nylon 6, a toughening agent, a lubricant, a nucleating agent and an antioxidant, and then carrying out plasticizing melting, extrusion and granulation to obtain the nylon 66 composite material.
9. The production method according to claim 8, wherein the plasticizing melting and extrusion are carried out in a twin-screw extruder, and the screw rotation speed is 200-350 rpm;
the machine barrel of the double-screw extruder is divided into 11 sections of temperature control areas from the blanking end to the machine head, and the temperature of each section of temperature control area is 265 ℃, 270 ℃, 265 ℃, 260 ℃, 265 ℃ and 270 ℃ in sequence.
10. Use of the nylon 66 composite material according to any one of claims 1 to 7 or the nylon 66 composite material prepared by the preparation method according to claim 8 or 9 in preparation of an automobile buckle.
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| CN112480665A (en) * | 2020-12-11 | 2021-03-12 | 上海金发科技发展有限公司 | High-fluidity high-impact-toughness nylon composite material and preparation method thereof |
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