CN116003999A - Low-warpage and easy-to-weld nylon composite material and preparation method thereof - Google Patents
Low-warpage and easy-to-weld nylon composite material and preparation method thereof Download PDFInfo
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- CN116003999A CN116003999A CN202211597424.1A CN202211597424A CN116003999A CN 116003999 A CN116003999 A CN 116003999A CN 202211597424 A CN202211597424 A CN 202211597424A CN 116003999 A CN116003999 A CN 116003999A
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- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000004952 Polyamide Substances 0.000 claims abstract description 46
- 229920002647 polyamide Polymers 0.000 claims abstract description 46
- 239000003365 glass fiber Substances 0.000 claims abstract description 25
- 238000002425 crystallisation Methods 0.000 claims abstract description 24
- 230000008025 crystallization Effects 0.000 claims abstract description 24
- 238000003466 welding Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 5
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- 229920005989 resin Polymers 0.000 claims description 8
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- 238000001035 drying Methods 0.000 claims description 7
- 229920006123 polyhexamethylene isophthalamide Polymers 0.000 claims description 7
- 101000576320 Homo sapiens Max-binding protein MNT Proteins 0.000 claims description 6
- 229920006121 Polyxylylene adipamide Polymers 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
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- 238000000034 method Methods 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 230000000655 anti-hydrolysis Effects 0.000 claims description 2
- 239000002216 antistatic agent Substances 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229920006177 crystalline aliphatic polyamide Polymers 0.000 claims description 2
- 239000004811 fluoropolymer Substances 0.000 claims description 2
- 229920002313 fluoropolymer Polymers 0.000 claims description 2
- 239000012760 heat stabilizer Substances 0.000 claims description 2
- 229910001510 metal chloride Inorganic materials 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 150000002989 phenols Chemical class 0.000 claims description 2
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000049 pigment Substances 0.000 claims description 2
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- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- SVUJNSGGPUCLQZ-FQQAACOVSA-N tenofovir alafenamide fumarate Chemical compound OC(=O)\C=C\C(O)=O.O([P@@](=O)(CO[C@H](C)CN1C2=NC=NC(N)=C2N=C1)N[C@@H](C)C(=O)OC(C)C)C1=CC=CC=C1.O([P@@](=O)(CO[C@H](C)CN1C2=NC=NC(N)=C2N=C1)N[C@@H](C)C(=O)OC(C)C)C1=CC=CC=C1 SVUJNSGGPUCLQZ-FQQAACOVSA-N 0.000 claims description 2
- 150000007970 thio esters Chemical class 0.000 claims description 2
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- 238000004381 surface treatment Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 10
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
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- 230000002787 reinforcement Effects 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- 125000003368 amide group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of nylon composite materials, in particular to a low-warpage and easy-welding nylon composite material and a preparation method thereof. Wherein, the nylon composite material with low warpage and easy welding comprises the following raw materials in percentage by mass: 23 to 70 percent of polyamide A, 5 to 25 percent of polyamide B, 20 to 50 percent of glass fiber, 0.1 to 0.5 percent of crystallization inhibitor, 0.1 to 0.6 percent of antioxidant, 0.1 to 0.6 percent of lubricant and 0 to 2 percent of other auxiliary agents. The low-warpage easy-welding nylon composite material provided by the invention is reinforced by adopting conventional cylindrical glass fibers, has better mechanical property and higher dimensional stability, has no floating fiber in appearance, is low in warpage, is easy to weld by a hot plate, has low cost, and can meet the application requirements of a filter, an automobile engine cover, a notebook computer and the like which not only require mechanical strength of the material, but also require large-sized parts with excellent apparent quality and good toughness.
Description
Technical Field
The invention relates to the technical field of nylon composite materials, in particular to a low-warpage and easy-welding nylon composite material and a preparation method thereof.
Background
The polyamide is a basic resin with the advantages of maximum yield, maximum variety, maximum application and excellent comprehensive performance in general engineering plastics, and has the advantages of good electric property, mechanical property, heat resistance, toughness, wear resistance, oil resistance, self-lubricating property, self-extinguishing property, chemical resistance, readily available raw materials, recycling, high cost performance and the like, so that the polyamide is widely used for replacing part of metal parts on automobiles, electronic appliances, household appliances, mechanical industry and the like to be matched with metals, and achieves the effects of reducing weight, friction coefficient and abrasion.
Although the polyamide has higher strength, abrasion resistance and self-lubricating property, the polyamide is easy to absorb water, the mechanical property is reduced after the polyamide absorbs water, the dimensional stability is poor, various problems are caused in the use process of the product, the stability of the material in use is required to be maintained through modification, and fiber reinforcement is a main way for solving the problems, and glass fiber reinforcement is most commonly used. However, due to the fact that the glass fiber orientation and the crystallization internal stress of the polyamide lead to inconsistent shrinkage of the melt in the flowing direction and the vertical flowing direction, the parts can be warped and deformed to influence assembly, and after the glass fiber is added, the fluidity of the material is reduced, and the appearance is easy to generate the problem of floating fiber.
At present, most patents and documents improve warpage by reducing glass fiber content and adding part of whisker, mica, talcum powder, wollastonite, glass microsphere and other inorganic minerals, such as Chinese patent 200710019484.4 discloses adding expandable graphite into a polyamide composite material, so that the fluidity of the material is improved and the warpage is reduced. Patent CN 1970629a discloses a resin and mica composite filling reinforcing material to improve the warp deformation of nylon; such methods can be effective in reducing warpage, but can directly result in reduced material properties, particularly impact properties.
Still other techniques improve warpage by using non-round section flat glass fiber, such as chinese patent CN200710306399, disclose a reinforced nylon with high glass fiber content achieved with a composition of flat glass fiber reinforced low viscosity polyamide, which has better flow properties and appearance, and can improve warpage. Patent 200810214041.5 discloses that the aromatic polyamide is reinforced with 40 to 80wt% of flat glass fiber, the fluidity of the material is improved, and the anisotropy is reduced. Patent CN114836030a discloses a low-warpage PA material and a preparation method thereof, and by adding a composite material of modified flat glass fiber and modified silicon dioxide, the warpage of nylon is effectively reduced, and meanwhile, the mechanical property of the nylon composite material is improved. Flat glass fibers are expensive and greatly limit the application of this method.
Therefore, it is an urgent problem to be solved how to obtain a polyamide material having good dimensional stability and strong mechanical properties while satisfying the requirements of the apparent mass.
Disclosure of Invention
In order to solve the defect that the existing polyamide material cannot meet the requirements of dimensional stability, mechanical property and apparent mass, the invention provides a low-warpage and easy-welding nylon composite material, which comprises the following raw materials in percentage by mass:
in some embodiments, the polyamide a is one or a mixture of several crystalline aliphatic polyamide resins having a faster crystallization rate, and the polyamide B has a smaller crystallization rate than the polyamide a.
In some embodiments, the polyamide a may be PA6 and/or PA66, and the relative viscosity of the polyamide a is 2.0 to 2.8.
In some embodiments, the polyamide B is amorphous transparent PA6I or MXD6 with a very slow crystallization rate.
In some embodiments, the glass fibers are plain round section alkali-free chopped glass fibers (E glass fibers) or continuous glass fibers that have been surface treated with a coupling agent, the glass fiber filaments having a diameter of 7 μm to 14 μm. Preferably, the glass fiber filaments have a diameter of 10 μm.
In some embodiments, the crystallization inhibitor is a metal chloride or rare earth.
Preferably, the crystallization inhibitor is anhydrous calcium chloride.
Preferably, the crystallization inhibitor is used in an amount of 0.2 to 0.4%.
In some embodiments, the antioxidant is one or more of hindered phenols, hindered amines, thioesters, phosphites, and complex antioxidants.
In some embodiments, the lubricant is any one or a combination of stearic acid, calcium stearate, stearate esters, TAF, silicone powder, PE wax, polyethylene glycol, fluoropolymers.
In some embodiments, the other processing aids include any one or combination of antistatic agents, coupling agents, heat stabilizers, anti-hydrolysis agents, plasticizers, pigments.
The preparation method of the low-warpage and easy-welding nylon composite material comprises the following steps:
drying the polyamide A and polyamide B resins in a dehumidifying dryer for 6 to 8 hours;
adding all the components except the glass fiber into a high-speed stirrer according to a proportion, and uniformly stirring to obtain premix;
and adding the premix into the double-screw extruder from a main feeding port, adding glass fibers into the double-screw extruder from a side feeding port, melting and extruding a material strip by adopting the double-screw extruder, cooling and drying, and cutting and granulating by a granulator to obtain the low-warpage and easy-welding nylon composite material.
Preferably, after drying, the moisture content of polyamide A and polyamide B is controlled to < 0.03%.
Preferably, the length-diameter ratio of the double-screw extruder is 40:1, the temperature range of the extruder is 220-290 ℃, and the screw rotating speed is 350-450 rpm; wherein the processing temperature of each section of the double-screw extruder is respectively as follows: the temperature of the first area is 150-200 ℃, the temperature of the second area is 230-290 ℃, the temperature of the third area is 230-290 ℃, the temperature of the fourth area is 230-290 ℃, the temperature of the fifth area is 230-290 ℃, the temperature of the sixth area is 230-290 ℃, the temperature of the seventh area is 230-290 ℃, the temperature of the eighth area is 230-290 ℃, the temperature of the ninth area is 230-290 ℃, the temperature of the tenth area is 240-290 ℃ and the temperature of the machine head is 240-290 ℃.
Based on the above, compared with the prior art, the invention has the following beneficial effects:
1. the low-warpage easy-welding nylon material provided by the invention adopts the polyamide B as amorphous transparent PA6I or MXD6 with very slow crystallization rate, the PA6I or MXD6 can interact with the polyamide A to reduce the crystallization rate, so that a molecular chain has longer relaxation time to release internal stress, and under the dual action of a crystallization inhibitor, the nylon crystallinity is reduced, the toughness is improved, the melting point is reduced, and then the warpage and the hot plate welding effect can be effectively improved.
2. According to the low-warpage easy-welding nylon material provided by the invention, the crystallization inhibitor shields hydrogen bonds among amide molecules through the complexation coordination reaction of metal ions and amide groups of nylon, so that nylon crystallization is hindered, toughness is improved, melting point is reduced, and warpage and hot plate welding effect can be improved.
3. The use amount of the crystallization inhibitor is too low, the crystallization inhibiting effect is not obvious, and the effect of improving the warpage and welding is not great, but when the use amount is too large, the crystallization damage is serious, and the mechanical strength and the heat resistance of the product are affected. The low-warpage easy-welding nylon material provided by the invention has the advantages that the benzene ring is contained on the PA6I or MXD6 molecular chain, the consumption of the crystallization inhibitor is regulated, so that the mechanical strength of the material is not reduced, the rigidity of the material is improved, the prepared nylon material has excellent performances of high strength, high toughness, low warpage, easy welding and the like, and the injection molding part has bright appearance and no floating fiber, and is suitable for automobile parts and electronic and electric products with high requirements on strength, toughness, appearance and warpage.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure and/or components pointed out in the written description and claims.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the following description will be made in conjunction with the technical solutions in the embodiments of the present invention, and it is apparent that the described embodiments are some, but not all, embodiments of the present invention; the technical features designed in the different embodiments of the invention described below can be combined with each other as long as they do not conflict with each other; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that all terms used in the present invention (including technical terms and scientific terms) have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs and are not to be construed as limiting the present invention; it will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
Drying the polyamide A and polyamide B resins in a dehumidifying dryer at 100 ℃ for 7 hours to enable the moisture content of the polyamide A and polyamide B resins to be less than 0.03%;
adding all the components except the glass fiber into a high-speed stirrer according to a proportion, and uniformly stirring to obtain premix;
and adding the premix into the double-screw extruder from a main feeding weightlessness type metering scale, adding glass fibers into the double-screw extruder from a side feeding weightlessness type metering scale, melting and extruding a material strip by adopting the double-screw extruder, cooling by a cooling water tank and drying by an air dryer, and then cutting and granulating by a granulator to obtain the low-warpage and easy-welding nylon composite material.
The length-diameter ratio of the double-screw extruder is 40:1, the temperature range of the extruder is 220-290 ℃, and the screw rotating speed is 350-450 rpm; wherein the processing temperature of each section of the double-screw extruder is respectively as follows: the temperature of the first area is 150-200 ℃, the temperature of the second area is 230-290 ℃, the temperature of the third area is 230-290 ℃, the temperature of the fourth area is 230-290 ℃, the temperature of the fifth area is 230-290 ℃, the temperature of the sixth area is 230-290 ℃, the temperature of the seventh area is 230-290 ℃, the temperature of the eighth area is 230-290 ℃, the temperature of the ninth area is 230-290 ℃, the temperature of the tenth area is 240-290 ℃ and the temperature of the machine head is 240-290 ℃.
The specific raw materials used in example 1 were as follows:
polyamide A1: PA66, supernatural horse EPR27
Polyamide A2: PA6, sea-sun HY2800A
Polyamide B1: MXD6, interference-fixed AP250
Polyamide B2, PA6I, east-west mountain Chen
Glass fiber: chongqing ECS301 CL
Crystallization inhibitor: anhydrous calcium chloride for national medicine group
An antioxidant: li Anlong 1098, li Anlong 168
And (3) a lubricant: honiswell AC540A.
The raw material ratios (the components in mass percent) of each example and comparative example provided by the invention are shown in table 1.
Table 1 raw material ratios of examples and comparative examples
Example 2
The components and preparation process were the same as in example 1, except that PA6 and PA66 were used for polyamide a. The mass ratio of PA6 to PA66 is 1:1.
Example 3
The components and preparation process were the same as in example 1, except that PA6I was used for polyamide B.
Example 4
The other components and preparation method are the same as in example 1 except for the adjustment of the proportion
Example 5
The other components and preparation method are the same as in example 1 except for the adjustment of the proportion
Comparative example 1
Except for the adjustment of the proportion, the other components and the preparation method were the same as in example 1.
Comparative example 2
Except for the adjustment of the proportion, the other components and the preparation method were the same as in example 1.
Comparative example 3
Except for the adjustment of the proportion, the other components and the preparation method were the same as in example 1.
Comparative example 4
Except for the adjustment of the proportion, the other components and the preparation method were the same as in example 1.
Comparative example 5
Except for the adjustment of the proportion, the other components and the preparation method were the same as in example 1.
Comparative example 6
Except for the adjustment of the proportion, the other components and the preparation method were the same as in example 1.
It should be noted that the specific parameters or some common reagents in the above embodiments are specific embodiments or preferred embodiments under the concept of the present invention, and are not limited thereto; and can be adaptively adjusted by those skilled in the art within the concept and the protection scope of the invention.
In addition, unless otherwise specified, the starting materials employed may also be commercially available products conventionally used in the art or may be prepared by methods conventionally used in the art.
The performance test, test items, standards and test results are shown in Table 2 for each example and comparative example.
Table 2 performance test tables for examples and comparative examples
As can be seen from Table 2, under the synergistic effect of polyamide B and a small-dose crystallization inhibitor, the warping degree of an injection molding product is obviously improved, the toughness is improved, the melting point is reduced, hot plate welding is facilitated, and when the using amount of the crystallization inhibitor adopted by the invention is controlled within a proportioning range, the mechanical property of the material is not obviously reduced, and meanwhile, the rigidity of the low-warping easy-welding nylon composite material provided by the application is improved under the action of benzene rings in a polyamide B molecular chain, and the prepared low-warping easy-welding nylon composite material has excellent performances such as high strength, high toughness, low warping, easy welding and the like.
In summary, compared with the prior art, the low-warpage easy-welding nylon composite material provided by the invention is reinforced by adopting the conventional cylindrical glass fiber, has better mechanical property and higher dimensional stability, has no floating fiber in appearance, is easy to weld by a hot plate, has low cost, and can meet the application requirements of a filter, an automobile engine cover, a notebook computer and the like, which not only require mechanical strength of the material, but also require large-sized products with excellent apparent quality and good toughness.
In addition, it should be understood by those skilled in the art that although many problems exist in the prior art, each embodiment or technical solution of the present invention may be modified in only one or several respects, without having to solve all technical problems listed in the prior art or the background art at the same time. Those skilled in the art will understand that nothing in one claim should be taken as a limitation on that claim.
Although terms such as polyamide a, polyamide B, glass fiber, crystallization inhibitor, antioxidant, lubricant, other auxiliary agent, etc. are more used herein, the possibility of using other terms is not excluded. These terms are used merely for convenience in describing and explaining the nature of the invention; they are to be interpreted as any additional limitation that is not inconsistent with the spirit of the present invention; the terms first, second, and the like in the description and in the claims, if any, are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The low-warpage and easy-welding nylon composite material is characterized by comprising the following raw materials in percentage by mass:
2. the low warp easy weld nylon composite of claim 1, wherein: the polyamide A is one or a mixture of a plurality of crystalline aliphatic polyamide resins with a faster crystallization rate, and the crystallization rate of the polyamide B is smaller than that of the polyamide A.
3. The low warp easy weld nylon composite of claim 2, wherein: the polyamide A can be PA6 and/or PA66, and the relative viscosity of the polyamide A is 2.0-2.8.
4. The low warp easy weld nylon composite of claim 1, wherein: the polyamide B is PA6I or MXD6.
5. The low warp easy weld nylon composite of claim 1, wherein: the glass fiber is common alkali-free chopped glass fiber or continuous glass fiber with circular cross section and subjected to surface treatment by a coupling agent.
6. The low warp easy weld nylon composite of claim 1, wherein: the crystallization inhibitor is metal chloride or rare earth.
7. The low warp easy weld nylon composite of claim 1, wherein: the antioxidant is one or more of hindered phenols, hindered amines, thioesters, phosphites and composite antioxidants.
8. The low warp easy weld nylon composite of claim 1, wherein: the lubricant is any one or combination of stearic acid, calcium stearate, TAF, silicone powder, PE wax, polyethylene glycol and fluoropolymer.
9. The low warp easy weld nylon composite of claim 1, wherein: the other processing aid comprises any one or combination of antistatic agent, coupling agent, heat stabilizer, anti-hydrolysis agent, plasticizer and pigment.
10. A method of preparing the low warpage easy welding nylon composite of any one of claims 1 to 9, comprising the steps of:
drying polyamide A and polyamide B resin, and controlling the water content to be less than 0.03%;
uniformly stirring all the components except the glass fiber in proportion to prepare a premix;
and respectively adding the premix and the glass fiber into a double-screw extruder, melting and extruding a material strip, cooling and drying, and cutting and granulating to obtain the low-warpage and easy-welding nylon composite material.
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