CN114716820B - A polyamide composition and its preparation method and application - Google Patents
A polyamide composition and its preparation method and application Download PDFInfo
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- CN114716820B CN114716820B CN202210226110.4A CN202210226110A CN114716820B CN 114716820 B CN114716820 B CN 114716820B CN 202210226110 A CN202210226110 A CN 202210226110A CN 114716820 B CN114716820 B CN 114716820B
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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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K5/00—Casings, cabinets or drawers for electric apparatus
- H05K5/02—Details
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
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Abstract
A polyamide composition is characterized by comprising, by weight, 50 parts of a polyamide resin, 30-65 parts of a reinforcing filler, 1-3 parts of a maleic anhydride grafted polyolefin, and an epoxy resin with an addition amount of 0.3-1.05 times that of the maleic anhydride grafted polyolefin, wherein the addition amount of the epoxy resin is not more than 2 parts. The invention can realize the advantage of high surface glossiness under the filling of a large amount of reinforcing filler through the compounding of the maleic anhydride grafted polyolefin and the epoxy resin.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polyamide composition, a preparation method and application thereof.
Background
Polyamide resins have excellent mechanical strength, heat resistance, chemical resistance, abrasion resistance and self-lubricating properties, and low friction coefficient, and are widely used in the fields of electronics and electricity, automobile parts, furniture, building materials, fibers and the like, and have become one of the most important engineering plastics. The reinforced polyamide resin has good mechanical properties and is expected to replace metal in a plurality of application fields, wherein the application fields comprise telecommunication, electronic consumer products, household appliances and shell materials of various motors and mechanical equipment. In these fields, it is desirable to have metal-like properties which can often only be achieved with highly filled, highly reinforced molding materials, in particular with high glass fiber content. However, the material with high glass fiber content inevitably leads to poor flowability and dispersibility of the material, so that the material is difficult to be smoothly injection-molded in thin walls and large parts, floating fiber on the injection-molded surface is serious, the requirement of the current electronic consumer products on high gloss of the shell material is difficult to be met, and meanwhile, the mechanical property is also influenced.
Improving the float appearance of high glass fiber content reinforced polyamides is generally accomplished by the following methods: 1. an amorphous polyamide resin, or a polyamide resin with a lower melting point, is added in a certain proportion to form an alloy of polyamide. 2. Adding a polyfunctional substance to form a branched polyamide composition, or directly adding a low molecular weight hyperbranched polyamide resin; 3. special types of glass fibers are used, such as non-round section profiled glass fibers or milled staple fibers. 4. With flow improvers or with low-viscosity polyamide resins.
EP0957131B1 describes improving the flow properties of polyamide compositions by adding polyamide prepolymers, but since the prepolymers have a very high concentration of end groups, subsequent reactions are unavoidable during the subsequent processing, which in turn leads to a reduction in the flow properties. Chinese patent CN1368994a discloses an improvement in the flowability of a high molecular weight polyamide composition by melt mixing a high molecular weight polyamide and a polyamide oligomer having a higher melting point than the high molecular weight polyamide at a melt temperature equal to or lower than the melting point, but this method is particularly limited and can only be effective in certain specific resin compositions where poor plasticization or non-melting of the oligomer occurs at the processing temperature of the high molecular weight matrix resin in some systems, such as in systems where improvement in the flowability of the high molecular weight PA6 material with PA66 oligomer. Chinese patent 200710306399 discloses a composition of low-viscosity polyamide reinforced by flat glass fibers, which realizes the reinforced composition of glass fiber content, has better flowability and injection molding surface quality, has smaller warpage, improves the traditional glass fiber reinforced material of surface quality, but has high cost and greatly limits the application of the method. In CN101193982B it is disclosed that linear or branched polyamide oligomers with a number average molar mass of 800-5000g/mol can effectively improve the processability and surface quality of high molecular weight polyamide materials, but that a separate polyamide oligomer end group adjustment step is required and the self strength of the material is also affected. Patent CN105419315A discloses a reinforced nylon composition with high glass fiber content, the nylon material contains 0.05-1% of star-shaped branching agent, the surface is improved by polyamide branching method, and the glossiness of the material is not high.
Disclosure of Invention
The invention aims to provide a polyamide composition with high glossiness, and a preparation method and application thereof.
The invention is realized by the following technical scheme:
a polyamide composition comprises, by weight, 50 parts of a polyamide resin, 30-65 parts of a reinforcing filler, 1-3 parts of a maleic anhydride grafted polyolefin, and an epoxy resin having a maleic anhydride grafted polyolefin content of 0.3-1.05 times, wherein the addition amount of the epoxy resin is not more than 2 parts.
Preferably, the epoxy resin is present in an amount of 0.6 to 0.8 times the maleic anhydride grafted polyolefin content.
The polyamide resin is at least one selected from PA6T/6I/66、PA6T/66、PA6I、PA6T/6I、PA6T/M5T、PA9T、PA9T/66、PA10T、PA10T/66、PA10T/10I、PA10T/1010、PA12T、PA12I、PA66、PA610、PA612、PA1010、PA1012、PA1212、PA6.
The reinforcing filler is at least one selected from carbon fiber, glass fiber, potassium titanate fiber, glass microsphere, glass flake, talcum powder, mica, clay, kaolin, silicon dioxide, silica fume, diatomite and calcium carbonate.
The maleic anhydride grafted polyolefin is at least one selected from maleic anhydride grafted polyethylene, maleic anhydride grafted polypropylene, maleic anhydride grafted ethylene propylene diene monomer rubber and maleic anhydride grafted ethylene octene copolymer;
Preferably, the maleic anhydride grafted polyolefin is selected from one of maleic anhydride grafted ethylene propylene diene monomer and maleic anhydride grafted ethylene octene copolymer.
The epoxy resin is at least one selected from bisphenol A epoxy resin, bisphenol F epoxy resin and glycidyl ester epoxy resin;
bisphenol a type epoxy resins are preferred.
Preferably, the epoxy resin has an epoxy equivalent weight in the range of 701-3000 g/eq; further preferably, the epoxy equivalent weight is in the range of 800 to 1000 g/eq.
In order to further improve the glossiness, at least one of 0-2 parts of dendritic polyamide is further included in parts by weight.
For example, a dendrimer is one of the dendrimers, which is a linear polymer with dendron units on each repeating unit. Dendritic units are highly branched structures containing very good geometric symmetry and a large number of surface functional groups. The highly branched structure of the dendritic units results in less intermolecular chain entanglement, with low melt viscosity characteristics. In addition, the regular arrangement of molecular chains can be reduced, so that the crystallization performance of the material is weakened. Dendritic polyamides are used in polyamide composites to facilitate providing flowability and improving surface appearance.
A process for preparing a polyamide composition comprising the steps of: according to the proportion, all components except the reinforcing filler are uniformly mixed, extruded and granulated by a double-screw extruder, the reinforcing filler is added by side feeding, and the temperature range of a screw is 270-330 ℃, so that the polyamide composition is obtained.
The application of the polyamide composition is used for preparing electronic product shells.
The invention has the following beneficial effects:
The invention utilizes the maleic anhydride grafted polyolefin with polar groups, can improve the interface combination between the reinforcing filler and the resin, can regulate the melt viscosity of the polyamide composition, is favorable for uniform dispersion of the filler, and further improves the mechanical property. Meanwhile, the maleic anhydride group and the epoxy group of the epoxy resin can react with the end group of the polyamide, so that the crystallinity and the crystallization rate of the polyamide resin can be regulated and controlled, and the dispersion of the filler is further improved. Further, the polyamide resin, the maleic anhydride grafted polyolefin and the epoxy resin which are reacted by the reaction can form a polymer net-shaped mixture, and a polymer surface layer with glossiness is formed on the surface of the product in the injection molding process, so that the composition can obtain very good surface glossiness.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
The sources of the raw materials used in the examples and comparative examples are as follows:
PA6T/6I/66: vicnyl 5300 NC003, jinfa technologies, inc.;
PA610: PA610-II, tin-free Yan Da;
PA66: PA66 EPR24, god Ma Jituan.
Glass fiber: commercially available, the same type of glass fiber was used in parallel experiments.
Talc powder: AH51215, liaoning Ai Hai;
Maleic anhydride grafted polyolefin a: maleic anhydride grafted PE, MC218 Ning wave energy photo New Material Co., ltd;
maleic anhydride grafted polyolefin B: maleic anhydride grafted PP, PC-3 new material of Nanhai cypress morning;
maleic anhydride grafted polyolefin C: maleic anhydride grafted EPDM, fusebond N416 dupont;
Maleic anhydride grafted polyolefin D: maleic anhydride grafted POE, fusebondn 493, dupont.
Epoxy resin a: bisphenol A type epoxy resin with epoxy equivalent weight of 875-975 and KD-214C is used in solid chemical industry;
Epoxy resin B: bisphenol F type epoxy resin with epoxy equivalent weight of 900-1000 and YDF-2004.
Epoxy resin C: bisphenol A type epoxy resin, epoxy equivalent weight, 1750-2100, YD-017 and solid chemical industry.
Epoxy resin D: bisphenol A type epoxy resin with epoxy equivalent weight of 600-700 and YD-012.
Epoxy resin E: bisphenol A epoxy resin with epoxy equivalent of 4100-6000 and YD-020 is used in chemical industry.
Dendritic polyamide: CYD-816A, wired morning original molecular New Material Co.
Preparation of polyamide compositions of examples and comparative examples: according to the proportion, all components except the reinforcing filler are uniformly mixed, extruded and granulated by a double-screw extruder, the reinforcing filler is added by side feeding, and the temperature range of a screw is 110-300-330-320-300-290-280-270-270-280-300-330 ℃, so that the polyamide composition is obtained.
The testing method comprises the following steps:
(1) 60 ° gloss: the sample plate dimensions were 60mm by 2.0mm and injection molded at a mold temperature of 100 ℃. Testing was performed according to the ISO 2813-2014 standard.
(2) Tensile strength: the measurement conditions were 23℃and 10mm/min according to ISO 527-2-2019;
(3) Notched Izod impact Strength: the test conditions were 23℃as determined according to ISO 180-2019.
Table 1: examples 1-7 Polyamide compositions component content (parts by weight) and test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| PA6T/6I/66 | 50 | 50 | 50 | 50 | 50 | ||
| PA610 | 50 | ||||||
| PA66 | 50 | ||||||
| Glass fiber | 30 | 30 | 30 | 30 | 40 | 50 | 65 |
| Maleic anhydride-grafted polyolefin D | 1 | 1 | 1 | 1.5 | 2 | 2.5 | 3 |
| Epoxy resin A | 0.5 | 0.5 | 0.5 | 0.75 | 1 | 1.25 | 2 |
| 60 Degree gloss | 86 | 90 | 87 | 86 | 86 | 83 | 81 |
| Tensile strength, MPa | 235 | 203 | 226 | 233 | 238 | 247 | 262 |
| Notched impact strength of cantilever beam, kJ/m 2 | 15.2 | 17.8 | 14.8 | 15.5 | 15.9 | 15.2 | 16.4 |
From examples 1 to 7, it is clear that the polyamide composition of the present invention has the advantage of high gloss.
Table 2: examples 8-11 Polyamide compositions component contents (parts by weight) and test results
| Example 8 | Example 9 | Example 10 | Example 11 | |
| PA6T/6I/66 | 50 | 50 | 50 | 50 |
| Glass fiber | 30 | 30 | 30 | 30 |
| Maleic anhydride-grafted polyolefin D | 1.5 | 1.5 | 1.5 | 1.5 |
| Epoxy resin A | 0.45 | 0.9 | 1.2 | 1.575 |
| 60 Degree gloss | 86 | 88 | 87 | 80 |
| Tensile strength, MPa | 235 | 232 | 228 | 215 |
| Notched impact strength of cantilever beam, kJ/m 2 | 15.3 | 15.5 | 15.8 | 16.6 |
As is clear from examples 4/8-11, the gloss is highest in the preferable range of the addition amount of the epoxy resin, and the mechanical properties can be maintained in a good range.
Table 3: examples 12-14 Polyamide compositions component contents (parts by weight) and test results
| Example 12 | Example 13 | Example 14 | |
| PA6T/6I/66 | 50 | 50 | 50 |
| Glass fiber | 30 | 30 | 30 |
| Maleic anhydride grafted polyolefin A | 1 | ||
| Maleic anhydride-grafted polyolefin B | 1 | ||
| Maleic anhydride-grafted polyolefin C | 1 | ||
| Epoxy resin A | 0.5 | 0.5 | 0.5 |
| 60 Degree gloss | 84 | 84 | 85 |
| Tensile strength, MPa | 228 | 226 | 237 |
| Notched impact strength of cantilever beam, kJ/m 2 | 13.5 | 13.8 | 14.9 |
As is evident from examples 1/12-14, maleic anhydride grafted POE and maleic anhydride grafted EPDM are preferred, not only for higher gloss, but also for better mechanical properties.
Table 4: examples 15-21 Polyamide compositions component contents (parts by weight) and test results
| Example 15 | Example 16 | Example 17 | Example 18 | Example 19 | Example 20 | Example 21 | |
| PA6T/6I/66 | 50 | 50 | 50 | 50 | 50 | 50 | 50 |
| Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
| Maleic anhydride-grafted polyolefin D | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| Epoxy resin B | 0.5 | 0.5 | 0.5 | 0.5 | |||
| Epoxy resin C | 0.5 | ||||||
| Epoxy resin D | 0.5 | ||||||
| Epoxy resin E | 0.5 | ||||||
| Dendritic polyamides | 0.1 | 1.0 | 2 | ||||
| 60 Degree gloss | 85 | 84 | 84 | 82 | 86 | 88 | 88 |
| Tensile strength, MPa | 226 | 233 | 229 | 241 | 232 | 230 | 227 |
| Notched impact strength of cantilever beam, kJ/m 2 | 15.9 | 15.3 | 14.6 | 16.2 | 15.4 | 15.1 | 14.8 |
As is clear from examples 1/15, the mechanical properties and gloss are both high from the bisphenol A type epoxy resin.
From examples 1/16 to 18, it is understood that the range of epoxy equivalent is preferable for the purpose of high gloss to have higher gloss and mechanical properties to be maintained at a high level. As is evident from examples 15/19-21, the gloss can be further improved by adding a dendritic polyamide.
Table 5: comparative example Polyamide composition content (parts by weight) and test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| PA6T/6I/66 | 50 | 50 | 50 | 50 | 50 | 50 |
| Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 |
| Maleic anhydride grafted polyolefin A | 1 | 2 | 1 | 0.5 | 3.5 | |
| Epoxy resin A | 0.5 | 2.1 | 0.2 | 0.1 | 2.5 | |
| 60 Degree gloss | 68 | 72 | 62 | 64 | 66 | 58 |
| Tensile strength, MPa | 224 | 222 | 213 | 234 | 232 | 203 |
| Notched impact strength of cantilever beam, kJ/m 2 | 13.6 | 12.4 | 16.8 | 15.4 | 14.9 | 17.9 |
As is clear from comparative example 1/2, the object of the present invention cannot be achieved by adding maleic anhydride-grafted polyolefin or epoxy resin alone.
As is clear from comparative example 3, when the addition amount of the epoxy resin is too high, a rapid decrease in gloss is caused instead.
As is clear from comparative example 4, when the addition amount of the epoxy resin is too low, the glossiness is low.
As is clear from comparative examples 5/6, when the addition amount of the maleic anhydride-grafted polyolefin is too low or too high, the purpose of high gloss cannot be achieved.
Claims (9)
1. A polyamide composition is characterized by comprising the following components in parts by weight: 50 parts of polyamide resin, 30-65 parts of reinforcing filler, 1-3 parts of maleic anhydride grafted polyolefin, wherein the content of epoxy resin is 0.3-0.8 times that of the maleic anhydride grafted polyolefin, but the addition amount of the epoxy resin is not more than 2 parts, and 0.1-2 parts of dendritic polyamide;
The epoxy equivalent weight of the epoxy resin is in the range of 800-1000g/eq.
2. The polyamide composition of claim 1 wherein the polyamide resin is selected from at least one of PA6T/6I/66、PA6T/66、PA6I、PA6T/6I、PA6T/M5T、PA9T、PA9T/66、PA10T、PA10T/66、PA10T/10I、PA10T/1010、PA12T、PA12I、PA66、PA610、PA612、PA1010、PA1012、PA1212、PA6.
3. The polyamide composition of claim 1, wherein the reinforcing filler is selected from at least one of carbon fiber, glass fiber, potassium titanate fiber, glass beads, glass flakes, talc, mica, clay, kaolin, silica fume, diatomaceous earth, and calcium carbonate.
4. The polyamide composition according to claim 1, wherein the maleic anhydride grafted polyolefin is at least one selected from the group consisting of maleic anhydride grafted polyethylene, maleic anhydride grafted polypropylene, maleic anhydride grafted ethylene propylene diene monomer, and maleic anhydride grafted ethylene octene copolymer.
5. The polyamide composition according to claim 1, wherein the maleic anhydride grafted polyolefin is one selected from the group consisting of maleic anhydride grafted ethylene propylene diene monomer and maleic anhydride grafted ethylene octene copolymer.
6. The polyamide composition according to claim 1, wherein the epoxy resin is at least one selected from the group consisting of bisphenol a type epoxy resin, bisphenol F type epoxy resin, and glycidyl ester type epoxy resin.
7. The polyamide composition of claim 1 wherein the epoxy resin is selected from bisphenol a type epoxy resins.
8. A process for the preparation of a polyamide composition according to any one of claims 1 to 7, characterized in that it comprises the following steps: according to the proportion, all components except the reinforcing filler are uniformly mixed, extruded and granulated by a double-screw extruder, the reinforcing filler is added by side feeding, and the temperature range of a screw is 270-330 ℃, so that the polyamide composition is obtained.
9. Use of a polyamide composition according to any one of claims 1 to 7 for the preparation of electronic housings.
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| CN103937231A (en) * | 2014-03-12 | 2014-07-23 | 金发科技股份有限公司 | Glass fiber reinforced nylon compound used for extrusion molding, and preparation method and application thereof |
| CN113817316A (en) * | 2021-08-12 | 2021-12-21 | 金发科技股份有限公司 | Semi-aromatic polyamide resin composition and preparation method and application thereof |
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| CN103937231A (en) * | 2014-03-12 | 2014-07-23 | 金发科技股份有限公司 | Glass fiber reinforced nylon compound used for extrusion molding, and preparation method and application thereof |
| CN113817316A (en) * | 2021-08-12 | 2021-12-21 | 金发科技股份有限公司 | Semi-aromatic polyamide resin composition and preparation method and application thereof |
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