CN115850967B - High-whiteness, high-heat-resistance and high-fluidity nylon composite material and preparation method thereof - Google Patents
High-whiteness, high-heat-resistance and high-fluidity nylon composite material and preparation method thereof Download PDFInfo
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- CN115850967B CN115850967B CN202211621925.9A CN202211621925A CN115850967B CN 115850967 B CN115850967 B CN 115850967B CN 202211621925 A CN202211621925 A CN 202211621925A CN 115850967 B CN115850967 B CN 115850967B
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- 239000004677 Nylon Substances 0.000 title claims abstract description 42
- 229920001778 nylon Polymers 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 34
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000010456 wollastonite Substances 0.000 claims abstract description 18
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000006081 fluorescent whitening agent Substances 0.000 claims abstract description 14
- 239000000314 lubricant Substances 0.000 claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 14
- 238000001125 extrusion Methods 0.000 claims description 20
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 12
- 229920006119 nylon 10T Polymers 0.000 claims description 12
- 229920006375 polyphtalamide Polymers 0.000 claims description 11
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical group [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 10
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 238000005282 brightening Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 229920006139 poly(hexamethylene adipamide-co-hexamethylene terephthalamide) Polymers 0.000 claims description 2
- -1 stilbene bisbenzimidazole Chemical group 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 235000010215 titanium dioxide Nutrition 0.000 abstract description 14
- 230000002087 whitening effect Effects 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004954 Polyphthalamide Substances 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a high-whiteness, high-heat-resistance and high-fluidity nylon composite material and a preparation method thereof, belonging to the field of polymer composite materials. The composite material comprises the following components in parts by weight: 55-70 parts of PPA, 15-25 parts of wollastonite, 10-25 parts of titanium dioxide, 0.02-0.1 part of fluorescent whitening agent, 0.2-0.9 part of antioxidant and 0.3-1 part of lubricant. The PPA with excellent fluidity and heat resistance is selected as a matrix material, a high-temperature-resistant antioxidant system formed by the mixed antioxidants is matched, and the assistants such as titanium white powder, high-temperature-resistant fluorescent whitening agent and the like with strong covering and whitening effects are adopted, so that the appearance of a high-temperature nylon product is remarkably improved, and the high-heat-resistant nylon material with high whiteness and good fluidity is prepared, and has important significance for development and application of the nylon material in the fields such as heat-resistant electrical appliance shells and the like.
Description
Technical Field
The invention relates to the technical field of polymer composite materials, in particular to a nylon composite material with high whiteness, high heat resistance and high fluidity and a preparation method thereof.
Background
After the molecular chain of the polyamide is introduced into the aromatic ring, the heat resistance and the mechanical property are greatly improved. Polyphthalamide (PPA, high temperature nylon) is a partially aromatic polyamide produced by taking terephthalic acid or isophthalic acid as a raw material, and is a typical high heat-resistant nylon material. The modified material has wide application prospect in the fields of electronics, electrics, automobiles, even military industry, aerospace and the like.
PPA (high temperature nylon) has strict requirements on whiteness of products when being applied to LED lamp brackets, heat-resistant electric appliance shells and the like. However, the processing temperature of high-temperature nylon is generally above 300 ℃, and thermooxidative aging is easy to occur during processing. Meanwhile, in order to improve the whiteness of the product, when a large amount of whitening additives such as titanium dioxide, zinc sulfide and the like are added, the integral fluidity of the system is extremely poor, and the high-temperature nylon product is extremely easily sheared and heated during extrusion and injection molding, so that the high-temperature nylon product becomes brittle and yellow, the formability in the extrusion process is poor, the appearance of the injection molding product is influenced, and the heat resistance is lost even after aging.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a nylon composite material with high whiteness, high heat resistance and high fluidity and a preparation method thereof.
The aim of the invention is realized by the following technical scheme:
The nylon composite material with high whiteness, high heat resistance and high fluidity comprises the following components in parts by weight:
wherein:
The PPA is at least one of nylon 10T/66 copolymer, nylon 9T/66 copolymer and nylon 6T/66 copolymer; the content of nylon 66 in the PPA is 45-60%.
The fiber diameter of the wollastonite is 10-19 microns, and the whiteness of the wollastonite is more than 88; specifically, the large interlinked ball wollastonite HQ1250, jiangxi Aote wollastonite AH-0028-03 or Jiangxi Aote wollastonite AH-BAKF can be selected.
The fluorescent whitening agent is a stilbene bisbenzimidazole compound KSN.
The antioxidant comprises at least one of an antioxidant 1098, an antioxidant Revonox 501, an antioxidant S-9228, an antioxidant Sumilizer S80 and an antioxidant TFB 117; further preferably, the antioxidant is an antioxidant 1098 and an antioxidant S-9228, and the weight ratio of the antioxidant to the antioxidant is 1: (1-3) a mixture;
The lubricant is zinc stearate.
The invention also provides a preparation method of the high-whiteness, high-heat-resistance and high-fluidity nylon composite material, which comprises the following steps:
(1) Uniformly mixing the dried PPA with titanium dioxide, a fluorescent whitening agent, an antioxidant and a lubricant according to a proportion to obtain a mixture;
(2) Adding the mixture into a double-screw extruder from a main feeding port, adding wollastonite into the double-screw extruder from a side feeding port, and carrying out melt extrusion and granulation to obtain the nylon material with high whiteness, high heat resistance and high fluidity. Preferably, the extrusion temperature of the twin-screw extruder is 290-330 ℃.
Compared with the prior art, the invention has the beneficial effects that:
The PPA with excellent fluidity and heat resistance is selected as a matrix material, a high-temperature-resistant antioxidant system consisting of an antioxidant 1098 and an antioxidant S-9228 is matched, and the assistants such as titanium white powder, a high-temperature-resistant fluorescent brightening agent and the like with strong covering and whitening effects are adopted, so that the appearance of a high-temperature nylon product is remarkably improved, and the prepared high-heat-resistant nylon material with high whiteness and good fluidity has important significance for development and application of the nylon material in the fields of heat-resistant electrical equipment shells and the like.
The raw materials used in the invention have sufficient sources, the process conditions are simple and stable, and excellent mechanical properties are maintained under the condition of realizing high whiteness of the product. The obtained product has good fluidity, easy processing and forming, stable size, good heat resistance and whiteness of more than 93 after being baked at the high temperature of 180 ℃ for 2 hours. The product can be widely applied to the fields of LED lamp brackets, heat-resistant electric appliance shells and the like.
Detailed Description
The present invention will be further described with reference to examples, which are not intended to be limiting, so that those skilled in the art will better understand the present invention and practice it.
In addition, the preparation processes in the following examples are conventional means in the art unless specifically described, and therefore, will not be described in detail; the parts in the following embodiments refer to parts by weight.
The types and suppliers of the reagents used in this example are as follows:
The nylon 10T/66 copolymer is H211MF produced by Huisheng New Material technology Co., ltd;
The titanium dioxide is DuPont titanium dioxide R105 in the United states;
Fluorescent whitening agent KSN and lubricant TFB 117 are derived from clariant;
wollastonite is HQ-1250 of the major interlinked ball mineral Co., ltd;
antioxidant 1098 is produced by basf;
The antioxidant S-9228 is chemically produced by Dufu;
Antioxidant Revonox 501 and antioxidant Sumilizer S80 are from Shanghai Pu Zhu Co., ltd;
The zinc stearate is from Anhui Shafeng New Material Co.
The above reagents are merely illustrative of the sources and ingredients of the reagents used in the experiments of the invention and are well disclosed and do not represent the inability to practice the invention using other reagents of the same type or provided by other suppliers.
Example 1:
a preparation method of a nylon composite material with high whiteness, high heat resistance and high fluidity comprises the following steps:
58 parts by weight of nylon 10T/66 copolymer, 22 parts by weight of titanium dioxide, 0.06 part by weight of fluorescent whitening agent, 0.35 part by weight of antioxidant 1098, 0.4 part by weight of antioxidant S-9228 and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer to be premixed for 10min, a double-screw extruder is added into a main feed opening, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feed opening, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is 180 ℃, three zones of 330 ℃, four zones of 320 ℃, five zones of 310 ℃, six zones of 295 ℃, seven zones of 295 ℃, eight zones of 290 ℃, nine zones of 300 ℃, ten zones of 310 ℃, and 320 ℃ of a machine head of the double-screw extruder, and the high-whiteness high-heat-resistance high-fluidity nylon material is obtained through melt extrusion and granulation.
Example 2:
a preparation method of a nylon composite material with high whiteness, high heat resistance and high fluidity comprises the following steps:
58 parts by weight of nylon 10T/66 copolymer, 22 parts by weight of titanium dioxide, 0.06 part by weight of fluorescent whitening agent, 0.35 part by weight of antioxidant Revonox 501, 0.4 part by weight of antioxidant Sumilizer S80 and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer to be premixed for 10min, a double-screw extruder is added into a main feed opening, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feed opening, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is 180 ℃, two zones 330 ℃, three zones 320 ℃, four zones 310 ℃, five zones 300 ℃, six zones 295 ℃, seven zones 295 ℃, eight zones 290 ℃, nine zones 300 ℃, ten zones 310 ℃, 320 ℃ and the head 320 ℃ are subjected to melt extrusion and granulation, so that the nylon material with high whiteness, high heat resistance and high fluidity is obtained.
Example 3:
a preparation method of a nylon composite material with high whiteness, high heat resistance and high fluidity comprises the following steps:
58 parts by weight of nylon 10T/66 copolymer, 22 parts by weight of titanium dioxide, 0.06 part by weight of fluorescent whitening agent, 0.35 part by weight of antioxidant TFB 117 and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer to be premixed for 10min, a double-screw extruder is added into a main blanking port, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feeding port, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is controlled to be 180 ℃, 330 ℃, 320 ℃, 310, 300 ℃, 295, 290 ℃, 300 ℃, 310, 320 ℃, 320, and granulating to obtain the nylon material with high whiteness, high heat resistance and high fluidity through melt extrusion.
Example 4:
a preparation method of a nylon composite material with high whiteness, high heat resistance and high fluidity comprises the following steps:
70 parts by weight of nylon 10T/66 copolymer, 10 parts by weight of titanium dioxide, 0.06 part by weight of fluorescent whitening agent, 0.35 part by weight of antioxidant TFB 117 and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer to be premixed for 10min, a double-screw extruder is added into a main blanking port, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feeding port, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is controlled to be 180 ℃, 330 ℃, 320 ℃, 310, 300 ℃, 295, 290 ℃, 300 ℃, 310, 320 ℃, 320, and granulating to obtain the nylon material with high whiteness, high heat resistance and high fluidity through melt extrusion.
The products prepared in the above examples were subjected to performance tests, the results of which are shown in Table 1 below:
TABLE 1
Note that: the color change of the material is characterized by a change db of a b value in the Lab color model, wherein the L value represents a brightness value, the b value is a color change from yellow to blue, and the db represents a change amount of the b value after baking for 2 hours.
Comparative example 1
The preparation method of the nylon composite material comprises the following steps:
After 58 parts by weight of nylon 10T/66 copolymer, 22 parts by weight of titanium dioxide, 0.06 part by weight of fluorescent whitening agent and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer for premixing for 10min, a double-screw extruder is added into a main feed opening, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feed opening, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is 180 ℃, two zones 325 ℃, three zones 320 ℃, four zones 310 ℃, five zones 300 ℃, six zones 295 ℃, seven zones 295 ℃, eight zones 295 ℃, nine zones 300 ℃, ten zones 310 ℃, a machine head 320 ℃, and the nylon composite material is obtained through melt extrusion and granulation.
Comparative example 2:
58 parts by weight of nylon 10T/66 copolymer, 22 parts by weight of titanium dioxide, 0.35 part by weight of antioxidant 1098, 0.4 part by weight of antioxidant S-9228 and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer to be premixed for 10min, a double-screw extruder is added into a main blanking port, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feeding port, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is controlled to be 180 ℃, 325 ℃, 320 ℃, 310, 300, 295, 300, 310, 320, and granulating to obtain the nylon composite material through melt extrusion.
Comparative example 3:
58 parts by weight of nylon 10T, 22 parts by weight of titanium dioxide, 0.35 part by weight of antioxidant 1098, 0.4 part by weight of antioxidant S-9228 and 0.8 part by weight of lubricant zinc stearate are placed in a high-speed mixer to be premixed for 10min, then a double-screw extruder is added into a main feed opening, 20 parts of wollastonite HQ-1250 is added into the double-screw extruder at a side feed opening, the rotating speed of the double-screw extruder is controlled to be 300rpm, the extrusion temperature of each zone is 180 ℃, 325 ℃, 320 ℃, 310 ℃, 300 ℃, 295 ℃, 300 ℃, 295, 300 ℃, 310 ℃, 320 ℃ and 320 ℃ of a machine head, and the nylon composite material is obtained through melt extrusion and granulation.
The products prepared in the above examples were subjected to performance tests, the results of which are shown in Table 2 below:
TABLE 2
Note that: the color change of the material is characterized by a change db of a b value in the Lab color model, wherein the L value represents a brightness value, the b value is a color change from yellow to blue, and the db represents a change amount of the b value after baking for 2 hours.
As can be seen from the results in tables 1 and 2, the material of comparative example 1 without antioxidant added, although the initial whiteness of the product is higher, the L value reaches 96.6, but under the condition of baking at 180 ℃ for 2 hours, the b value is changed from-0.98 to 1.82, and the yellowing of the product is more serious; the initial whiteness of the product of the material without the fluorescent whitening agent in comparative example 2 is lower and only reaches 92.9. This shows that the combination of the antioxidant components, especially the antioxidant 1098 and the antioxidant S-9228 in the embodiment 1, can effectively improve the baking yellowing resistance of the high-temperature nylon product, and the addition of the fluorescent whitening agent KSN can effectively improve the whiteness of the high-temperature nylon product; in comparative example 3, homopolymerized PA10T is selected, and the injection fluidity deviation shows that after nylon 10T is copolymerized by nylon 66, the fluidity of the product is greatly improved.
It will be apparent that the described embodiments are some, but not all, embodiments of the invention. 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.
Claims (5)
1. A nylon composite material with high whiteness, high heat resistance and high fluidity is characterized in that: the composition by weight fraction is as follows:
55-70 parts of PPA,
15-25 Parts of wollastonite,
10-25 Parts of titanium dioxide,
0.02-0.1 Part of fluorescent brightening agent,
0.2 To 0.9 part of antioxidant,
0.3-1 Part of lubricant;
the antioxidant is an antioxidant 1098 and an antioxidant S-9228, and the weight ratio of the antioxidant to the antioxidant is 1: (1-3) a mixture;
The PPA is at least one of nylon 10T/66 copolymer, nylon 9T/66 copolymer and nylon 6T/66 copolymer; the content of nylon 66 in the PPA is 45-60%;
the fluorescent whitening agent is a stilbene bisbenzimidazole compound KSN.
2. The high whiteness, high heat resistance, high fluidity nylon composite according to claim 1, characterized in that: the wollastonite has a fiber diameter of 10-19 microns.
3. The high whiteness, high heat resistance, high fluidity nylon composite according to claim 1, characterized in that: the lubricant is zinc stearate.
4. A method for producing a high whiteness, high heat resistance, high fluidity nylon composite material according to any one of claims 1 to 3, characterized in that: the method comprises the following steps:
(1) Uniformly mixing the dried PPA with titanium dioxide, a fluorescent whitening agent, an antioxidant and a lubricant according to a proportion to obtain a mixture;
(2) Adding the mixture into a double-screw extruder from a main feeding port, adding wollastonite into the double-screw extruder from a side feeding port, and carrying out melt extrusion and granulation to obtain the nylon material with high whiteness, high heat resistance and high fluidity.
5. The method for preparing the high-whiteness, high-heat-resistance and high-fluidity nylon composite material according to claim 4, which is characterized in that: the extrusion temperature of the double-screw extruder is 290-330 ℃.
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| CN202211621925.9A CN115850967B (en) | 2022-12-16 | High-whiteness, high-heat-resistance and high-fluidity nylon composite material and preparation method thereof |
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| CN202211621925.9A CN115850967B (en) | 2022-12-16 | High-whiteness, high-heat-resistance and high-fluidity nylon composite material and preparation method thereof |
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| CN115850967B true CN115850967B (en) | 2024-06-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104710780A (en) * | 2013-12-16 | 2015-06-17 | 上海杰事杰新材料(集团)股份有限公司 | Ceramic whisker enhanced high-temperature-resistant nylon composite material and preparation method thereof |
| CN108285640A (en) * | 2017-12-26 | 2018-07-17 | 浙江普利特新材料有限公司 | A kind of resisting high-temperature yellowing nylon material and preparation method thereof |
| CN115260758A (en) * | 2022-08-24 | 2022-11-01 | 横店集团得邦工程塑料有限公司 | High-reflectivity heat-aging-resistant PA10T material and preparation method thereof |
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710780A (en) * | 2013-12-16 | 2015-06-17 | 上海杰事杰新材料(集团)股份有限公司 | Ceramic whisker enhanced high-temperature-resistant nylon composite material and preparation method thereof |
| CN108285640A (en) * | 2017-12-26 | 2018-07-17 | 浙江普利特新材料有限公司 | A kind of resisting high-temperature yellowing nylon material and preparation method thereof |
| CN115260758A (en) * | 2022-08-24 | 2022-11-01 | 横店集团得邦工程塑料有限公司 | High-reflectivity heat-aging-resistant PA10T material and preparation method thereof |
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