CN115216141A - High-gloss high-glass-fiber reinforced PA6 material and preparation method thereof - Google Patents
High-gloss high-glass-fiber reinforced PA6 material and preparation method thereof Download PDFInfo
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- CN115216141A CN115216141A CN202210957325.3A CN202210957325A CN115216141A CN 115216141 A CN115216141 A CN 115216141A CN 202210957325 A CN202210957325 A CN 202210957325A CN 115216141 A CN115216141 A CN 115216141A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
Abstract
The invention belongs to the technical field of high polymer material processing, and discloses a high-gloss high-glass-fiber reinforced PA6 material and a preparation method thereof. The high-gloss high-glass-fiber reinforced PA6 material comprises, by weight, 30-50 parts of PA6 resin, 5-10 parts of MXD6 resin, 40-60 parts of glass fiber, 0.5-5 parts of modified petroleum resin, 0.1-0.5 part of antioxidant and 0.1-0.3 part of heat stabilizer. The composite material takes PA6 resin as a base material, poly m-xylylene adipamide is compounded according to a certain proportion, and then high-strength S glass fiber is compounded and reinforced; meanwhile, the modified hydrogenated petroleum resin C9-g-MAH with a certain proportion is added into the formula, so that the wettability of the composite material can be improved, the bonding strength between polyamide and glass fiber can be improved, and the material has good surface appearance; and then compounding with components such as an antioxidant, a heat stabilizer and the like, so that the weather resistance of the material is improved, and the finally obtained glass fiber reinforced PA6 material has excellent physical properties, injection molding appearance and heat aging resistance.
Description
Technical Field
The invention relates to the technical field of high polymer material processing, in particular to a high-gloss high-glass-fiber reinforced PA6 material and a preparation method thereof.
Background
The traditional electric appliance bracket material is generally made of metal materials, and a die-casting process is adopted, but the metal materials have high specific gravity and high cost, can generate larger heat in the processing process, and is contrary to the current policies related to low-carbon emission and carbon neutralization. The plastic is used for replacing steel in the current hot door direction, the high polymer material has lower processing temperature, the carbon emission amount in the processing process is less, after the composite modification is carried out on the high polymer material, the integral rigidity strength can be greatly improved, and the performance of some special materials can even approach to that of metal materials.
The PA6 resin has good mechanical processing characteristics, excellent chemical resistance and other characteristics, and the strength, the hardness, the fatigue resistance, the dimensional stability, the creep resistance and the like of the PA6 resin are greatly improved after the PA6 resin is reinforced and modified by Glass Fibers (GF). However, the dispersibility and bonding strength of the glass fibers in the nylon PA resin matrix greatly affect the product performance, and after the glass fibers are added, the toughness of the composite material is reduced, and the brittleness is increased; the glass fiber can be oriented along the flow direction in the injection molding process, so that the mechanical property and the shrinkage rate are enhanced in the orientation direction, and the product is deformed and warped; in addition, during the injection molding process, the glass fibers enter the surface of the plastic product, so that the surface of the product becomes rough, and spots, such as defects of floating fibers, material flowers and the like, are formed. Meanwhile, the glass fiber content of the traditional glass fiber reinforced PA6 material is generally controlled to be 10-40%, the existence of the higher glass fiber content enables the material to have higher rigidity strength, but the defects of glass fiber exposure, warping and the like are amplified. Therefore, the development of the glass fiber reinforced PA6 material with high performance and high glossiness, which is suitable for the electric appliance bracket, has important application significance.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provide a high-gloss high-glass-fiber reinforced PA6 material and a preparation method thereof, wherein the composite material takes PA6 resin as a base material and is compounded with semi-aromatic crystalline polyamide resin (polycide) in a certain proportionM-xylylene amide), enhanced by high-strength S-glass fiber, and simultaneously added with modified petroleum resin C 9 -g-MAH, and then compounding with components such as an antioxidant, a heat stabilizer and the like, so that the finally obtained glass fiber reinforced PA6 material has excellent physical properties, injection molding appearance and thermal aging resistance.
In order to achieve the purpose of the invention, the high-gloss high-glass-fiber reinforced PA6 material comprises, by weight, 30-50 parts of PA6 resin, 5-10 parts of MXD6 resin, 40-60 parts of glass fiber, 0.5-5 parts of modified petroleum resin, 0.1-0.5 part of antioxidant and 0.1-0.3 part of heat stabilizer.
Further, in some embodiments of the present invention, the PA6 resin is a PA6 resin having a viscosity ranging between 2.0-2.5.
Further, in some embodiments of the invention, the MXD6 resin is polycaproylm-xylylenediamine, a semi-aromatic crystalline polyamide resin, commonly referred to as "nylon MXD6" for short.
Further, in some embodiments of the present invention, the glass fibers are S-glass fibers having a higher silica content than ordinary E-glass fibers.
Further, in some embodiments of the invention, the modified petroleum resin is maleic anhydride modified petroleum resin C 9 -g-MAH。
Further, in some embodiments of the present invention, the antioxidant is a combination of hindered phenolic antioxidant and phosphite ester-based auxiliary antioxidant, and preferably, the mass ratio of the hindered phenolic antioxidant to the phosphite ester-based auxiliary antioxidant is 1:1-3.
Further, in some embodiments of the present invention, the thermal stabilizer is a copper salt stabilizer.
On the other hand, the invention also provides a preparation method of the high-gloss high-glass-fiber reinforced PA6 material, which comprises the following steps:
(1) Weighing PA6 resin, MXD6 resin, modified petroleum resin, glass fiber, antioxidant and heat stabilizer according to the required weight parts for later use;
(2) Adding the PA6 resin and the MXD6 resin into a stirrer, then adding the modified petroleum resin, the antioxidant and the heat stabilizer, and stirring uniformly at normal temperature;
(3) And (3) placing the mixed material obtained in the step (2) into a co-rotating double-screw extruder, and carrying out melt plastification, extrusion, cooling and grain cutting to obtain the high-gloss high-glass-fiber reinforced PA6 material, wherein the glass fiber is added in a side feeding manner in the extrusion section process.
Further, in some embodiments of the present invention, the co-rotating twin screw extruder has a screw diameter of 40 to 65mm, a screw length to diameter ratio of 40:1.
further, in some embodiments of the invention, the melt plastication temperature is set to 230 ℃ to 250 ℃ in the first section, 230 ℃ to 250 ℃ in the second section, 230 ℃ to 250 ℃ in the third section, 220 ℃ to 240 ℃ in the fourth section, 220 ℃ to 240 ℃ in the fifth section, 220 ℃ to 240 ℃ in the sixth section, 220 ℃ to 240 ℃ in the seventh section, 220 ℃ to 240 ℃ in the eighth section, 220 ℃ to 240 ℃ in the ninth section, 220 ℃ to 240 ℃ in the tenth section, 230 ℃ to 250 ℃ in the melt temperature, and 240 ℃ to 260 ℃ in the head.
Compared with the prior art, the invention has the following advantages:
(1) The high-gloss high-glass-fiber reinforced PA6 material disclosed by the invention is compounded with MXD6 resin in a certain proportion, so that the crystallization temperature and the crystallization speed of a composite system are reduced, and the MXD6 resin is slow in cooling speed in a melt state, is easy to coat on the surfaces of glass fibers and PA6 components, and is very favorable for improving the surface gloss of the material. Meanwhile, MXD6 is coated on the surface of the material, and the excellent barrier property of the material plays a good role in isolating oxygen, so that the thermal-oxidative aging of the material is delayed, and the thermal aging resistance of the composite material is greatly enhanced.
(2) The high-gloss high-glass-fiber reinforced PA6 material is reinforced by high-strength S glass fibers, and compared with E glass fibers, the high-gloss high-glass-fiber reinforced PA6 material has higher silicon dioxide content, and the prepared composite material has higher tensile strength, elastic modulus and rigidity.
(3) The high-gloss high-glass-fiber reinforced PA6 material is added with maleic anhydride modified petroleum resin C in a certain proportion 9 -g-MAH, petroleum tree modified with terminal functional groups, having a low molecular weight and good fluidityFat C 9 the-g-MAH has good polarity, has good compatibility with other components of the composite material, can improve the wettability of the composite material and the bonding strength between polyamide and glass fiber, and simultaneously the resin can float on the surface of the composite material in a melt state to form a bright resin film, so that the appearance of the material is very bright.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains" or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of 8230comprises" excludes any non-specified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of 8230title" appears in a clause of the subject matter of the claims and not immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
The indefinite articles "a" and "an" preceding an element or component of the invention are used without limitation to the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
Furthermore, the description below of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. In addition, the technical features according to the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Examples
A high-gloss high-glass-fiber reinforced PA6 material comprises the following components in parts by weight:
the specific materials and weight parts are given in Table 1.
Wherein the PA6 resin has a viscosity ranging from 2.0 to 2.5The PA6 resin of (1); the MXD6 resin is polyhexamethylene isophthalamide which is a semi-aromatic crystalline polyamide resin generally referred to as nylon MXD6 for short; the glass fiber is a high-strength S glass fiber; the modified petroleum resin is maleic anhydride modified petroleum resin C 9 -g-MAH; the antioxidant is a combination of hindered phenol antioxidant and phosphite ester auxiliary antioxidant, and the mass ratio is 1; the heat stabilizer is a copper salt stabilizer.
The materials of examples 1-4 and comparative examples 1-4 were prepared as follows:
(1) Weighing PA6 resin, MXD6 resin, modified petroleum resin, high-strength S glass fiber, antioxidant and heat stabilizer in required weight parts for later use;
(2) Adding the PA6 resin and the MXD6 resin into a stirrer, then adding the modified petroleum resin, the antioxidant and the copper salt stabilizer, and stirring uniformly at normal temperature;
(3) And (3) placing the mixed material obtained in the step (2) into a co-rotating double-screw extruder, and carrying out melt plasticizing, extrusion, cooling and grain cutting to obtain the high-gloss high-glass-fiber reinforced PA6 material, wherein the high-strength S glass fiber is added in a side feeding manner in the extrusion section process.
The diameter of the screw of the co-rotating twin-screw extruder used in the method can be 40-65mm, and the length-diameter ratio of the screw is 40:1, setting the melt plasticizing temperature to 230-250 ℃ in the first section, 230-250 ℃ in the second section, 230-250 ℃ in the third section, 220-240 ℃ in the fourth section, 220-240 ℃ in the fifth section, 220-240 ℃ in the sixth section, 220-240 ℃ in the seventh section, 220-240 ℃ in the eighth section, 220-240 ℃ in the ninth section, 220-240 ℃ in the tenth section, 230-250 ℃ in the melt temperature and 240-260 ℃ in the head. Within these parameters, the properties of the prepared materials are almost the same.
TABLE 1 specific formulation of materials (in kilograms) for examples 1-4 and comparative examples 1-4
The PA6 composite materials obtained in the examples and the comparative examples are dried in a 120 ℃ oven and then are subjected to injection molding to form sample pieces, and the injection molding temperature is as follows:
a blanking section: 250 ℃; and a second stage: 255 ℃; a third stage: 275 ℃; a nozzle: 275 ℃.
And finally, placing the injection molding sample wafer in a dryer for state adjustment: adjusting the temperature to 23 ℃ and the adjusting time to 24h; the results of the performance tests on the materials of the examples and comparative examples are shown in table 2 below.
Table 2 results of property test of materials of examples and comparative examples
From the test results of example 1 and comparative example 3, it can be seen that: modified Petroleum resin C 9 The g-MAH is beneficial to improving the surface gloss of the material in a composite system. Is due to C 9 The g-MAH has good polarity and good compatibility with other components in the composite material, and meanwhile, the resin can float on the surface of the composite material in a melt state to form a layer of bright resin film, so that the appearance of the material is extremely bright.
From the test results of comparative example 1 and comparative example 2, it can be seen that: the MXD6 can improve the rigidity and the strength of the material, reduce the warping degree of the material, improve the surface gloss of the material and the like. The reason is that the addition of MXD6 can reduce the crystallization temperature and the crystallization speed of a composite system, the MXD6 is slow in cooling speed in a melt state, is easy to coat on the surfaces of glass fibers and PA6 components, is very favorable for improving the surface gloss of the material, and the lower crystallinity can reduce the warping severity of the material.
From the test results of comparative example 1 and comparative example 3, it can be seen that: the reinforcing effect of the high-strength S glass fiber in the composite material is far higher than that of the common E glass fiber.
Placing the injection molding sample wafer in a hot oven for thermal aging test, adopting the standard of GB/T7141-2008, setting the temperature to be 150 +/-5, and testing time: 1000h, 3000h, and the results of the performance tests of the materials of the examples and comparative examples after the tests are shown in tables 3-4 below.
TABLE 3 1000h Performance test results of 150 ℃ thermal aging test
TABLE 4 3000h Performance test results of 150 deg.C thermal aging test
As can be seen from the results of the heat aging tests of examples 1 to 4 and comparative examples 1 to 4: the performance of the group added with the MXD6 is much slower than that of the group not added in a thermal aging test, and the change of the unnotched impact performance is particularly reflected, so that the MXD6 is coated on the surface of the material, and the excellent barrier property of the MXD6 plays a good role in isolating oxygen, thereby delaying the thermal aging of the material and greatly enhancing the thermal aging resistance of the composite material.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.
Claims (10)
1. The high-gloss high-glass-fiber reinforced PA6 material is characterized by comprising 30-50 parts by weight of PA6 resin, 5-10 parts by weight of MXD6 resin, 40-60 parts by weight of glass fiber, 0.5-5 parts by weight of modified petroleum resin, 0.1-0.5 part by weight of antioxidant and 0.1-0.3 part by weight of heat stabilizer.
2. The high-gloss high-glass-fiber reinforced PA6 material as claimed in claim 1, wherein the high-gloss high-glass-fiber reinforced PA6 material comprises, by weight, 30-45 parts of PA6 resin, 5-10 parts of MXD6 resin, 50-60 parts of glass fiber, 1-3 parts of modified petroleum resin, 0.1-0.5 part of antioxidant and 0.1-0.3 part of heat stabilizer.
3. The high gloss high fiberglass reinforced PA6 material of claim 1, wherein said PA6 resin is a PA6 resin having a viscosity ranging between 2.0-2.5.
4. The high gloss high fiberglass reinforced PA6 material of claim 1, wherein said glass fibers are S-glass fibers.
5. The high gloss high fiberglass reinforced PA6 material according to claim 1, wherein said modified petroleum resin is maleic anhydride modified petroleum resin C 9 -g-MAH。
6. The high-gloss high-glass-fiber reinforced PA6 material as claimed in claim 1, wherein the antioxidant is a combination of hindered phenolic antioxidant and phosphite ester auxiliary antioxidant, and preferably the mass ratio of the hindered phenolic antioxidant to the phosphite ester auxiliary antioxidant is 1:1-3.
7. The high gloss high fiberglass reinforced PA6 material of claim 1, wherein said thermal stabilizer is a copper salt stabilizer.
8. The process for preparing a high gloss high glass fiber reinforced PA6 material according to any of claims 1 to 7, characterized in that the process comprises the steps of:
(1) Weighing PA6 resin, MXD6 resin, modified petroleum resin, glass fiber, antioxidant and heat stabilizer in required parts by weight for later use;
(2) Adding the PA6 resin and the MXD6 resin into a stirrer, then adding the modified petroleum resin, the antioxidant and the heat stabilizer, and stirring uniformly at normal temperature;
(3) And (3) placing the mixed material obtained in the step (2) into a co-rotating double-screw extruder, and carrying out melt plastification, extrusion, cooling and grain cutting to obtain the high-gloss high-glass-fiber reinforced PA6 material, wherein the glass fiber is added in a side feeding manner in the extrusion section process.
9. The method for preparing the high-gloss high-glass-fiber reinforced PA6 material according to claim 8, wherein the diameter of a screw of the co-rotating twin-screw extruder is 40-65mm, and the length-diameter ratio of the screw is 40:1.
10. the method for preparing the high-gloss high-glass-fiber reinforced PA6 material according to claim 8, wherein the melt plasticizing temperature is set to 230-250 ℃ in the first section, 230-250 ℃ in the second section, 230-250 ℃ in the third section, 220-240 ℃ in the fourth section, 220-240 ℃ in the fifth section, 220-240 ℃ in the sixth section, 220-240 ℃ in the seventh section, 220-240 ℃ in the eighth section, 220-240 ℃ in the ninth section, 220-240 ℃ in the tenth section, 230-250 ℃ in the melt temperature, and 240-260 ℃ in the head section.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116875045A (en) * | 2023-05-12 | 2023-10-13 | 江苏金发科技新材料有限公司 | Glass fiber reinforced nylon material and preparation method thereof |
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