CN114716820A - Polyamide composition and preparation method and application thereof - Google Patents
Polyamide composition and preparation method and application thereof Download PDFInfo
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- CN114716820A CN114716820A CN202210226110.4A CN202210226110A CN114716820A CN 114716820 A CN114716820 A CN 114716820A CN 202210226110 A CN202210226110 A CN 202210226110A CN 114716820 A CN114716820 A CN 114716820A
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- maleic anhydride
- epoxy resin
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- polyamide
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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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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The polyamide composition is characterized by comprising 50 parts of polyamide resin, 30-65 parts of reinforcing filler, 1-3 parts of maleic anhydride grafted polyolefin and epoxy resin with the addition amount of 0.3-1.05 times that of the maleic anhydride grafted polyolefin in parts by weight, wherein the addition amount of the epoxy resin is not higher than 2 parts. According to the invention, through compounding of the maleic anhydride grafted polyolefin and the epoxy resin, the advantage of high surface gloss can be realized under the filling of a large amount of reinforcing filler.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polyamide composition and a preparation method and application thereof.
Background
Polyamide resins have excellent mechanical strength, heat resistance, chemical resistance, abrasion resistance, self-lubricity, and a low coefficient of friction, and are widely used in the fields of electronics and electronics, 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 metals in a plurality of application fields, including housing materials of telecommunication, electronic consumer goods, household appliances and various motors and mechanical equipment. In these fields, there is a need for metal-like properties which are often only achievable by highly filled, highly reinforced molding materials, especially high glass fiber content reinforced molding materials. However, the material with high glass fiber content inevitably causes poor material fluidity and dispersibility, smooth injection molding is difficult for some thin-wall and large parts, fiber floating on the injection molding surface is serious, the requirement of the current electronic consumer goods on high gloss of the shell material is difficult to meet, and the mechanical property is also influenced.
The appearance of the floating fiber of the high glass fiber content reinforced polyamide is improved by the following methods: 1. a proportion of amorphous polyamide resin, or a lower melting polyamide resin, is added to form an alloy of polyamide. 2. Adding a multifunctional 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 profiled glass fibers of non-circular cross-section or milled staple fibers. 4. With flow improvers or with low-viscosity polyamide resins.
EP0957131B1 describes the improvement of the flow properties of polyamide compositions by the addition of polyamide prepolymers, but owing to the high concentration of end groups in the prepolymer, subsequent reactions are unavoidable in the later processing, which in turn lead to a reduction in the flow properties. Chinese patent CN1368994A discloses a method for improving the flowability of high molecular weight polyamide compositions 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 only effective in certain specific resin compositions, and in some systems poor plasticization or no melting of the oligomer occurs at the processing temperature of the high molecular weight matrix resin, such as occurs in systems where the flowability of the high molecular weight PA6 material is improved with PA66 oligomer. Chinese patent 200710306399 discloses a composition of flat glass fiber reinforced low viscosity polyamide, which realizes a glass fiber content reinforced composition, has better flow property and injection molding surface quality, has less warpage, and has improved surface quality compared with the conventional glass fiber reinforced material, but has high cost, thus greatly limiting the application of the method. Patent CN101193982B discloses that linear or branched polyamide oligomers having a number average molar mass of 800-5000g/mol are effective in improving the processability and surface quality of high molecular weight polyamide materials, but require a separate polyamide oligomer end group conditioning step and the strength of the material itself is affected. Patent CN105419315A discloses a high glass fiber content reinforced nylon composition, wherein the nylon material contains 0.05-1% of star 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 polyamide resin, 30-65 parts of reinforcing filler, 1-3 parts of maleic anhydride grafted polyolefin and epoxy resin with the maleic anhydride grafted polyolefin content being 0.3-1.05 times, wherein the addition amount of the epoxy resin is not higher than 2 parts.
Preferably, the content of the epoxy resin is 0.6 to 0.8 times the content of the maleic anhydride-grafted polyolefin.
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 and PA 6.
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, wollastonite, 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 one selected from maleic anhydride grafted ethylene propylene diene monomer rubber and maleic anhydride grafted ethylene octene copolymer.
The epoxy resin is selected from at least one of bisphenol A epoxy resin, bisphenol F epoxy resin and glycidyl ester epoxy resin;
bisphenol a type epoxy resins are preferred.
Preferably, the epoxy equivalent of the epoxy resin is in the range of 701-3000 g/eq; further preferably, the epoxy equivalent is in the range of 800-1000 g/eq.
In order to further improve the glossiness, at least one of 0-2 parts of dendritic polyamide is also included by weight.
By way of example, a dendritic polyamide is one of the dendritic polymers, which is a linear polymer with dendron units on each repeating unit. The dendritic unit is of a highly branched structure and contains good geometric symmetry and a large number of surface functional groups. The highly branched structure of the dendritic unit allows less intermolecular chain entanglement and has a low melt viscosity characteristic. In addition, the regular arrangement of molecular chains can be reduced, thereby weakening the crystallization performance of the material. Dendritic polyamides are used in polyamide composites to help provide flow and improve surface appearance.
A process for preparing a polyamide composition comprising the steps of: according to the proportion, the components except the reinforced filler are uniformly mixed, and are extruded and granulated by a double-screw extruder, the reinforced filler is added by side feeding, and the temperature range of a screw is 270 ℃ plus 330 ℃, so that the polyamide composition is obtained.
The polyamide composition is applied to preparing electronic product shells.
The invention has the following beneficial effects:
the invention can improve the interface combination between the reinforced filler and the resin by grafting the polyolefin with the maleic anhydride with the polar group, and can adjust the melt viscosity of the polyamide composition, thereby being beneficial to the uniform dispersion of the filler and further improving 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 can form a polymer network mixture, and a polymer surface layer with glossiness is formed on the surface of a workpiece in the injection molding process, so that the composition obtains 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 invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw material sources used in the examples and comparative examples are as follows:
PA 6T/6I/66: vicyl 5300 NC003, King-Korea technologies, Inc.;
PA 610: PA610-II, tin-free Yinda;
PA 66: PA66 EPR24, suma group.
Glass fiber: commercially available, parallel experiments were performed using the same glass fibers.
Talc powder: AH51215, aisheng aihai;
maleic anhydride-grafted polyolefin a: new photo materials Co., Ltd of maleic anhydride grafted PE, MC218 Nile energy;
maleic anhydride-grafted polyolefin B: PP grafted by maleic anhydride, and a new material PC-3 south China sea cypress;
maleic anhydride-grafted polyolefin C: maleic anhydride grafted EPDM, FUSABOND N416 dupont;
maleic anhydride-grafted polyolefin D: maleic anhydride grafted POE, fusabond 493, dupont.
Epoxy resin A: bisphenol A type epoxy resin, epoxy equivalent 875-;
epoxy resin B: bisphenol F type epoxy resin, epoxy equivalent of 900-.
Epoxy resin C: bisphenol A epoxy resin, epoxy equivalent, 1750-2100, YD-017, all chemical engineering.
Epoxy resin D: bisphenol A type epoxy resin, the epoxy equivalent of 600-700, YD-012, solid chemical industry.
Epoxy resin E: bisphenol A type epoxy resin, epoxy equivalent 4100-.
Dendritic polyamide: CYD-816A, Waishaham molecular materials Innova.
Examples and comparative examples preparation of polyamide compositions: according to the proportion, the components except the reinforcing filler are uniformly mixed, and are extruded and granulated by a double-screw extruder, the reinforcing filler is added by side feeding, and the screw temperature range is 110-.
The test methods are as follows:
(1) 60 ° gloss: the sample size was 60mm × 60mm × 2.0mm, and injection molding was performed at a mold temperature of 100 ℃. The test was performed according to ISO 2813-2014 standard.
(2) Tensile strength: measured according to ISO 527-2-2019, the measuring condition is 23 ℃, 10 mm/min;
(3) notched izod impact strength: the test conditions were 23 ℃ determined according to ISO 180-2019.
Table 1: examples 1-7 Polyamide compositions with respective component contents (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 polyolefins 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 Izod impact Strength, kJ/m2 | 15.2 | 17.8 | 14.8 | 15.5 | 15.9 | 15.2 | 16.4 |
From examples 1 to 7, it can be seen that the polyamide compositions of the invention have the advantage of high gloss.
Table 2: examples 8-11 Polyamide compositions with respective 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 polyolefins 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 Izod impact Strength, kJ/m2 | 15.3 | 15.5 | 15.8 | 16.6 |
From examples 4/8-11, it is understood that the gloss is highest and the mechanical properties can be maintained in a good range within the preferable range of the amount of the epoxy resin added.
Table 3: examples 12-14 Polyamide compositions with respective component amounts (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 polyolefins C | 1 | ||
| Epoxy resin A | 0.5 | 0.5 | 0.5 |
| 60 degree gloss | 84 | 84 | 85 |
| Tensile strength, MPa | 228 | 226 | 237 |
| Notched Izod impact Strength, kJ/m2 | 13.5 | 13.8 | 14.9 |
As can be seen from examples 1/12-14, maleic anhydride grafted POE and maleic anhydride grafted EPDM are preferred, which not only provide higher gloss, but also provide better mechanical properties.
Table 4: examples 15 to 21 Polyamide compositions with respective 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 polyolefins 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 Izod impact Strength, kJ/m2 | 15.9 | 15.3 | 14.6 | 16.2 | 15.4 | 15.1 | 14.8 |
From example 1/15, it is clear that the bisphenol A type epoxy resin is preferable, and the mechanical properties and the gloss are high.
From examples 1/16 to 18, it is understood that the gloss is higher in the preferred epoxy equivalent range and the mechanical properties can be maintained at a high level for the purpose of high gloss. From examples 15/19 to 21, it is clear that the addition of the dendritic polyamide can further improve the gloss.
Table 5: comparative example Polyamide composition Components 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 Izod impact Strength, kJ/m2 | 13.6 | 12.4 | 16.8 | 15.4 | 14.9 | 17.9 |
As can be seen from comparative example 1/2, the addition of maleic anhydride-grafted polyolefin or epoxy resin alone did not achieve the object of the present invention.
From comparative example 3, it is understood that when the amount of the epoxy resin added is too high, a rapid decrease in gloss is caused instead.
From comparative example 4, it is understood that when the amount of the epoxy resin added is too low, the gloss is low.
It is understood from comparative example 5/6 that when the amount of addition of the maleic anhydride-grafted polyolefin is too low or too high, the object of high gloss is not achieved.
Claims (10)
1. The polyamide composition is characterized by comprising 50 parts of polyamide resin, 30-65 parts of reinforcing filler, 1-3 parts of maleic anhydride grafted polyolefin and epoxy resin with the content of 0.3-1.05 times that of the maleic anhydride grafted polyolefin by weight, wherein the addition amount of the epoxy resin is not higher than 2 parts.
2. Polyamide composition according to claim 1, characterized in that the content of epoxy resin is 0.6-0.8 times the content of maleic anhydride grafted polyolefin.
3. The polyamide composition according to claim 1, wherein the polyamide resin is at least one selected from the group consisting 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, and PA 6.
4. The polyamide composition as claimed in claim 1, wherein the reinforcing filler is at least one selected from the group consisting of carbon fibers, glass fibers, potassium titanate fibers, glass microspheres, glass flakes, talc, mica, clay, kaolin, silica, wollastonite, diatomaceous earth and calcium carbonate.
5. 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 rubber, and maleic anhydride grafted ethylene octene copolymer, and preferably, the maleic anhydride grafted polyolefin is one selected from the group consisting of maleic anhydride grafted ethylene propylene diene monomer rubber, 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 a bisphenol a type epoxy resin, a bisphenol F type epoxy resin, and a glycidyl ester type epoxy resin; bisphenol a type epoxy resins are preferred.
7. The polyamide composition as claimed in claim 6, wherein the epoxy resin has an epoxy equivalent weight in the range of 701-3000 g/eq; preferably 800-1000 g/eq.
8. The polyamide composition of claim 1, further comprising at least one of 0 to 2 parts by weight of a dendritic polyamide.
9. Process for the preparation of a polyamide composition according to any one of claims 1 to 8, characterized in that it comprises the following steps: according to the proportion, the components except the reinforced filler are uniformly mixed, and are extruded and granulated by a double-screw extruder, the reinforced filler is added by side feeding, and the temperature range of a screw is 270 ℃ plus 330 ℃, so that the polyamide composition is obtained.
10. Use of a polyamide composition according to any one of claims 1 to 8 for the preparation of housings for electronic products.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115746552A (en) * | 2022-10-12 | 2023-03-07 | 金发科技股份有限公司 | Nylon composite material and preparation method and application thereof |
| CN116478534A (en) * | 2023-04-28 | 2023-07-25 | 金发科技股份有限公司 | Wear-resistant PA composition and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101193982A (en) * | 2005-05-20 | 2008-06-04 | Ems-化学公开股份有限公司 | Polyamide molding materials with an improved flowability, the production thereof and its use |
| 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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2022
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101193982A (en) * | 2005-05-20 | 2008-06-04 | Ems-化学公开股份有限公司 | Polyamide molding materials with an improved flowability, the production thereof and its use |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115746552A (en) * | 2022-10-12 | 2023-03-07 | 金发科技股份有限公司 | Nylon composite material and preparation method and application thereof |
| CN115746552B (en) * | 2022-10-12 | 2024-03-26 | 金发科技股份有限公司 | Nylon composite material and preparation method and application thereof |
| CN116478534A (en) * | 2023-04-28 | 2023-07-25 | 金发科技股份有限公司 | Wear-resistant PA composition and preparation method and application thereof |
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