CN111961336A - Infrared-transmitting polyamide composition and preparation method thereof - Google Patents
Infrared-transmitting polyamide composition and preparation method thereof Download PDFInfo
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention provides an infrared-transmitting polyamide composition and a preparation method thereof, wherein the composition is prepared from the following raw materials in parts by weight: 57-88 parts of polyamide resin, 10-30 parts of polyetherimide, 1-5 parts of compatilizer, 0.1-0.3 part of infrared transmission improver and 0.1-1 part of processing aid. The infrared-transmitting polyamide composition has excellent flame retardant property, transparency and infrared-transmitting effect, the infrared-transmitting property of the composition is greatly improved by adding the infrared-transmitting improving agent, the application range of the composition is widened, the composition can be used under visible light, the infrared-transmitting requirement is met at night, and the composition can be better applied to military industry and medical science.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to an infrared-permeable polyamide composition and a preparation method thereof.
Background
Polyamide (PA), also known as nylon, was commercialized in 1939. With the development of industrial technology, transparent nylon is gradually applied to the market, has the inherent characteristics of nylon, including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubrication, has low friction coefficient, is easy to process, is suitable for being filled with glass fiber and other fillers for reinforcing and modifying, but cannot achieve the transparent effect after reinforcing and flame-retardant modification in some special fields, so that the application of the transparent nylon is limited.
The polyetherimide is an amber transparent high polymer material and has high temperature resistance, solvent resistance, radiation resistance, hydrolysis resistance, flame retardant property and the like. The excellent performance enables the application range to be wider, for example, some parts with higher temperature resistance are manufactured, the excellent electrical insulation performance can be applied to the field of electronics and electricity, the use temperature is 180-200 ℃, and the injection molding temperature is 330 ℃. In particular, the good flame retardant property of the flame retardant is applied to some service environments with fire prevention requirements.
In the fields of security, mineral production, oil exploitation and the like, for the requirement of safety, high temperature resistance and the requirements of transparency and fire resistance are required under certain high-temperature environments, the traditional flame-retardant material is adopted, the traditional flame-retardant material is not high in heat resistance, most of the fireproof materials are opaque, the polyetherimide material is adopted, the fireproof grade of the polyetherimide material can meet the requirements, but amber has certain influence on the transparency of the polyetherimide material, and the transparent nylon has good performances of oil resistance, heat resistance and the like and cannot meet the requirement of fire resistance, so that any one material used independently is difficult to meet the application of the current market. If the transparent nylon and polyetherimide material are used as alloy materials, the alloy material not only can meet the requirements of high heat resistance and fire resistance, but also has the unique performance advantage of transparency, and the alloy of the material is rarely reported at present.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects in the prior art and provide an infrared-transmitting polyamide composition and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
an infrared-transmitting polyamide composition is prepared from the following raw materials in parts by weight:
preferably, the composition is prepared from the following raw materials in parts by weight:
further, the polyamide resin is transparent polyamide; the light transmittance of the polyamide resin is more than or equal to 90 percent; the polyamide resin is polyamide with the carbon chain length between adjacent amide groups being greater than or equal to 10.
Further, the polyetherimide is formed by condensation polymerization of bisphenol A type diether dianhydride and diamine monomer; the diamine is prepared by copolymerizing phenylenediamine and propane diamine, wherein the molar ratio of the phenylenediamine to the propane diamine is 1-4: 1. the polyamide resin is polyetherimide superfine powder.
Further, the compatilizer is at least one of N-methyl pyrrolidone, dimethyl sulfoxide, N-dimethylacetamide or N, N-dimethylformamide; preferably, the compatilizer is N-methyl pyrrolidone. The N-methyl pyrrolidone enables the material to have high polarity and reactivity, and can greatly improve the compatibility of the composite material. The compatibilizer is the polar aprotic solvent.
Further, the infrared transmission improving agent is a mixture of zinc selenide and at least one of zinc oxide or zinc sulfide, and the mass ratio of the zinc selenide in the mixture is more than 50%. The zinc selenide is nano-grade zinc selenide and is prepared by a vapor deposition method under the protection of nitrogen.
Further, the processing aid is at least one of an antioxidant or a coupling agent; the antioxidant is a compound of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylene diamine and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite; the coupling agent is a silane coupling agent containing amino.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
Further, in the step (2), the temperature of the first zone of the twin-screw extruder is 250-minus 270 ℃, the temperature of the second zone is 260-minus 280 ℃, the temperature of the third zone is 260-minus 280 ℃, the temperature of the fourth zone is 260-minus 280 ℃, the temperature of the fifth zone is 270-minus 290 ℃, the temperature of the sixth zone is 280-minus 300 ℃, the temperature of the seventh zone is 270-minus 290 ℃, the temperature of the eighth zone is 260-minus 280 ℃, the temperature of the ninth zone is 240-minus 260 ℃, the retention time is 1-3 minutes, and the rotation speed of the host machine is 250-minus 350 revolutions per minute.
Reduction of the viscosity of Polyetherimide (PEI) with silicone oil: the PEI is filled with the hydroxyl silicone oil, the hydroxyl silicone oil can be combined with the viscous components in the PEI, even a clathrate compound is formed, so that the quantity of the viscous components of the PEI system is reduced, the viscosity of the PEI system is reduced, the reduced PEI is fully bonded with the silicone oil for later use at a certain temperature, and thus the subsequent dispersibility of the PEI and the nylon is facilitated, and the processability of the composition is improved.
Compared with the prior art, the invention has the following advantages:
the infrared-transmitting polyamide composition has excellent flame retardant property, transparency and infrared-transmitting effect, the infrared-transmitting property of the composition is greatly improved by adding the infrared-transmitting improving agent, the application range of the composition is widened, the composition can be used under visible light, the infrared-transmitting requirement is met at night, and the composition can be better applied to military industry and medical science.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
In the examples and comparative examples described in the present invention: the polyamide resin is PA12, Trogamid CX series of Evonik company; selection of Mitsubishi chemical for polyetherimides
U1000; the compatilizer is N-methylpyrrolidone (NMP); the infrared transmission improving agent is nano high-purity zinc selenide (the purity is 99.99 percent) sold in the market, and the zinc oxide is nano zinc oxide; the antioxidant is IRGANOX1098 produced and sold by Ciba.
The present invention will be described in detail with reference to examples.
Example 1
An infrared-transmitting polyamide composition is prepared from the following raw materials in parts by weight: 81.8 parts of polyamide resin, 15 parts of polyetherimide, 3 parts of compatilizer, 0.1 part of infrared transmission improver and 0.1 part of antioxidant.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 2
An infrared-transmitting polyamide composition is prepared from the following raw materials in parts by weight: 66.8 parts of polyamide resin, 30 parts of polyetherimide, 3 parts of compatilizer, 0.1 part of infrared transmission improving agent and 0.1 part of antioxidant.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 3
An infrared-transmitting polyamide composition is prepared from the following raw materials in parts by weight: 66.7 parts of polyamide resin, 30 parts of polyetherimide, 3 parts of compatilizer, 0.2 part of infrared transmission improving agent and 0.1 part of antioxidant.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 4
An infrared-transmitting polyamide composition is prepared from the following raw materials in parts by weight: 66.7 parts of polyamide resin, 30 parts of polyetherimide, 3 parts of compatilizer, 0.3 part of infrared transmission improving agent and 0.1 part of antioxidant.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Example 5
An infrared-transmitting polyamide composition is prepared from the following raw materials in parts by weight: 56.6 parts of polyamide resin, 40 parts of polyetherimide, 3 parts of compatilizer, 0.3 part of infrared transmission improver and 0.1 part of antioxidant.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
Comparative example 1
The polyamide composition is prepared from the following raw materials in parts by weight: 84.9 parts of polyamide resin, 15 parts of polyetherimide and 0.1 part of antioxidant.
The preparation method of the infrared-transmitting polyamide composition comprises the following steps: the preparation method comprises the steps of uniformly mixing polyamide resin, polyetherimide and an antioxidant in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, cooling, drying and dicing after extrusion to obtain the polyamide resin.
In the step (2), the temperature of the first zone of the double-screw extruder is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 270 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the seventh zone is 280 ℃, the temperature of the eighth zone is 270 ℃, the temperature of the ninth zone is 250 ℃, the residence time is 1-3 minutes, and the rotating speed of the main machine is 250-.
And (3) putting the prepared granules into a blast oven, drying for 4h at the temperature of 130 ℃, and then injecting the dried granules into an injection molding machine for molding sample strips. The injection molding mold temperature was 60 ℃. The performance test criteria for the infrared-permeable polyamide compositions obtained according to the invention are shown in table 1.
Table 1 test items of physical and mechanical properties of materials and corresponding test methods
| Test items | Test method and conditions |
| Light transmittance | GBT 2410-2008/1mm |
| Limiting oxygen index | GB2406 |
| Heat distortion temperature | GB1634/ISO 75/1.82MPa |
| Glass transition temperature | GB19466 |
| Infrared transmission test | GB6040 |
The physical properties of the infrared-transmitting polyamide compositions obtained in examples 1 to 5 and comparative example 1 are shown in Table 2.
TABLE 2 physical Properties of Infrared permeable Polyamide compositions
As can be seen from Table 3, the infrared-transmitting polyamide composition has excellent infrared-transmitting and visible light-transmitting properties, flame retardant properties and light transmittance, and the use range of the composition is widened by adding the infrared-transmitting improving agent, and the composition is simple to manufacture and convenient to realize and can be used in military industry, medicine and current new technology VR and AR products used for transmitting infrared. But also can be used in the field of fire safety, and makes up the blank of using under the condition of simultaneously requiring fire prevention and infrared transmission at present.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. An infrared-transmissive polyamide composition characterized by: the composition is prepared from the following raw materials in parts by weight:
2. the infrared permeable polyamide composition of claim 1, wherein: the composition is prepared from the following raw materials in parts by weight:
3. the infrared permeable polyamide composition of claim 1, wherein: the polyamide resin is transparent polyamide; the light transmittance of the polyamide resin is more than or equal to 90 percent; the polyamide resin is polyamide with the carbon chain length between adjacent amide groups being greater than or equal to 10.
4. The infrared permeable polyamide composition of claim 1, wherein: the polyetherimide is prepared by condensation polymerization of bisphenol A type diether dianhydride and diamine monomer; the diamine is prepared by copolymerizing phenylenediamine and propane diamine, wherein the molar ratio of the phenylenediamine to the propane diamine is 1-4: 1.
5. the infrared permeable polyamide composition of claim 1, wherein: the compatilizer is at least one of N-methyl pyrrolidone, dimethyl sulfoxide, N-dimethylacetamide or N, N-dimethylformamide; preferably, the compatilizer is N-methyl pyrrolidone.
6. The infrared permeable polyamide composition of claim 1, wherein: the infrared transmission improving agent is a mixture of zinc selenide and at least one of zinc oxide or zinc sulfide, and the mass ratio of the zinc selenide in the mixture is more than 50%.
7. The infrared permeable polyamide composition of claim 1, wherein: the processing aid is at least one of an antioxidant or a coupling agent; the antioxidant is a compound of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylene diamine and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite; the coupling agent is a silane coupling agent containing amino.
8. Process for the preparation of an infrared-permeable polyamide composition according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
(1) filling hydroxyl silicone oil into the polyetherimide, and fully bonding to obtain a polyetherimide mixture;
(2) and (2) uniformly mixing polyamide resin, the polyetherimide mixture obtained in the step (1), the infrared transmission improving agent, the compatilizer and the processing aid in a high-speed mixer, adding the obtained mixed material into a double-screw extruder from a main feeding port, and cooling, drying and granulating after extrusion to obtain the polyether imide.
9. The method of preparing an infrared-transmissive polyamide composition as recited in claim 8, wherein: in the step (2), the temperature of the first zone of the twin-screw extruder is 250-.
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| US4657987A (en) * | 1984-01-27 | 1987-04-14 | General Electric Company | Polyetherimide-polyamide blends |
| CN103627066A (en) * | 2013-11-27 | 2014-03-12 | 安徽科聚新材料有限公司 | Far infrared ray transmitting composite material and preparation method thereof |
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| CN106243710A (en) * | 2016-08-30 | 2016-12-21 | 聚威工程塑料(上海)有限公司 | A kind of infrared through fiber glass reinforced polyamide 66 |
| CN107974079A (en) * | 2017-12-12 | 2018-05-01 | 天津金发新材料有限公司 | A kind of nylon/ABS alloy composite material and preparation method thereof |
| CN108884315A (en) * | 2016-02-22 | 2018-11-23 | 巴斯夫欧洲公司 | Black daiamid composition and its preparation and use |
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2020
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|---|---|---|---|---|
| US4657987A (en) * | 1984-01-27 | 1987-04-14 | General Electric Company | Polyetherimide-polyamide blends |
| CN103627066A (en) * | 2013-11-27 | 2014-03-12 | 安徽科聚新材料有限公司 | Far infrared ray transmitting composite material and preparation method thereof |
| CN104497560A (en) * | 2014-12-11 | 2015-04-08 | 江苏金发科技新材料有限公司 | Polyamide flame-retardant composition and preparation method thereof |
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| CN105057594A (en) * | 2015-07-30 | 2015-11-18 | 宁波天业精密铸造有限公司 | Precise investment casting technology |
| CN108884315A (en) * | 2016-02-22 | 2018-11-23 | 巴斯夫欧洲公司 | Black daiamid composition and its preparation and use |
| CN106243710A (en) * | 2016-08-30 | 2016-12-21 | 聚威工程塑料(上海)有限公司 | A kind of infrared through fiber glass reinforced polyamide 66 |
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