CN115433448B - Polycarbonate composition and preparation method and application thereof - Google Patents
Polycarbonate composition and preparation method and application thereof Download PDFInfo
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- CN115433448B CN115433448B CN202211061336.XA CN202211061336A CN115433448B CN 115433448 B CN115433448 B CN 115433448B CN 202211061336 A CN202211061336 A CN 202211061336A CN 115433448 B CN115433448 B CN 115433448B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
- C08K2003/3036—Sulfides of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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Abstract
The invention discloses a polycarbonate composition, which comprises the following components in percentage by weight: 97.2% -99.7% of polycarbonate resin; 0.1% -1.5% of optical functional substance; 0.1% -0.5% of an acidic treating agent; 0.1 to 0.8 percent of antioxidant. According to the polycarbonate composition, a certain amount of optical functional substances, an acidic treatment agent and an antioxidant are added, and all the components are synergistic, so that the material has special optical properties of selective infrared transmission (the infrared light transmittance at 850nm with the thickness of 1.5mm is higher than 27%, the visible light transmittance at 550nm is lower than 15%), meanwhile, high thermal stability can be kept, the material can still keep high toughness (the notch impact strength of a cantilever beam is higher than 650J/m) after being subjected to heat treatment at 320 ℃ for 10min, and the application requirements of special optical devices such as an indicator lamp, a remote controller or wearing equipment can be particularly met.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polycarbonate composition and a preparation method and application thereof.
Background
The Polycarbonate (PC) has the characteristics of colorless transparency, heat resistance, impact resistance, high light transmittance and good optical performance, is a thermoplastic engineering plastic with excellent comprehensive performance, fully utilizes the transparency of the material, and has good application prospect on some special optical devices. The infrared ray penetrating PC material refers to a material capable of penetrating infrared radiation, has the characteristics of long wavelength, strong penetrating capacity, high energy and the like, and is widely applied to the fields of signal transmission, energy transmission and the like. The existing infrared transmission PC material is mainly modified by adding an infrared transmission material into a polycarbonate material, and Chinese patent application CN112724630A discloses an infrared transmission flame-retardant polycarbonate composition, and by adding a certain proportion of magnesium fluoride and calcium sulfate, the infrared transmission rate is improved, and meanwhile, the visible light transmission rate is reduced to a certain extent. However, the ester group structure in the PC molecular chain is extremely easy to cause the breakage of the molecular chain after being treated at high temperature under the existence of alkaline substances, so that the material is degraded, the mechanical property is seriously degraded, and the use is influenced. Most of the current infrared transmitting PC materials are under study for their special optical properties, while few related studies are being conducted on how to improve the thermal stability properties of the infrared transmitting PC materials.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a high-heat-stability special optical polycarbonate composition, which has an infrared light transmittance of more than 27% and a visible light transmittance of less than 15% at a thickness of 1.5mm (the interference of visible light on signals can be reduced while the signal transmission effect of infrared light is maintained), and can still maintain higher toughness after high-temperature treatment.
It is another object of the present invention to provide a method for producing the above polycarbonate composition.
The invention is realized by the following technical scheme:
a polycarbonate composition comprising the following components in weight percent:
97.2% -99.7% of polycarbonate resin;
0.1% -1.5% of optical functional substance;
0.1% -0.5% of an acidic treating agent;
0.1 to 0.8 percent of antioxidant.
Preferably, the polycarbonate composition comprises the following components in percentage by weight:
97.8% -99.0% of polycarbonate resin;
0.6% -1.2% of optical functional substance;
0.2% -0.4% of an acidic treating agent;
0.2 to 0.6 percent of antioxidant.
Preferably, the number average molecular weight of the polycarbonate resin is 18000-40000; more preferably, the polycarbonate resin has a number average molecular weight of 25000 to 38000.
The optical functional substance is selected from any one or more of titanium dioxide, talcum powder, zinc sulfide, zinc oxide, magnesium oxide, calcium carbonate, vermiculite, halloysite or wollastonite; preferably, the optical functional object is selected from any one or more of titanium dioxide, zinc oxide or zinc sulfide; more preferably, the optical functional material is selected from titanium dioxide. The optical functional object adopted by the invention can effectively shield the transmission of visible light, and has little influence on the infrared light transmittance.
The acidic treating agent is selected from any one or more of oxidized polyethylene grafted maleic anhydride, oxidized polyethylene wax or ethylene-vinyl acetate copolymer. Preferably, the acidic treatment agent is selected from oxidized polyethylene grafted maleic anhydride.
More preferably, the acid value of the acidic treating agent is 20 to 60mgKOH/g. The acid number is the milligrams of potassium hydroxide consumed in titrating each gram of sample.
The antioxidant is selected from any one or more of hydroxylated thiodiphenyl ethers, alkylated monophenols or polyphenols, polyalcohols, bis (2, 6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphate, tris (2, 4-di-tert-butylphenyl) phosphite or pentaerythritol tetra (3-laurylthiopropionate).
Preferably, the antioxidant is selected from any one or more of bis (2, 6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphate, tris (2, 4-di-tert-butylphenyl) phosphite, pentaerythritol tetra (3-laurylthiopropionate) or hydroxylated thiodiphenyl ethers.
The invention also provides a preparation method of the polycarbonate composition, which comprises the following steps: adding the components into a high-speed mixer according to the proportion, and uniformly mixing to obtain a premix; then, putting the obtained premix into a double-screw extruder for melt mixing, extruding and granulating to prepare a polycarbonate composition; wherein the length-diameter ratio of the double-screw extruder is 40:1-48:1; the temperature of the twin-screw extruder was set at 230-300 ℃.
The invention also provides application of the polycarbonate composition in an indicator lamp, a remote controller or wearable equipment
The invention has the following beneficial effects:
according to the polycarbonate composition, a certain amount of optical functional substances, an acidic treatment agent and an antioxidant are added, and all the components are synergistic, so that the material has special optical properties of selective infrared transmission (the infrared light transmittance at 850nm with the thickness of 1.5mm is higher than 27%, the visible light transmittance at 550nm is lower than 15%), meanwhile, high thermal stability can be kept, the material can still keep high toughness (the notch impact strength of a cantilever beam is higher than 650J/m) after being subjected to heat treatment at 320 ℃ for 10min, and the application requirements of special optical devices such as an indicator lamp, a remote controller or wearing equipment can be particularly met.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
The raw materials used in the examples and comparative examples of the present invention are described below, but are not limited to these materials:
polycarbonate resin 1: number average molecular weight 28000, S-2000F, mitsubishi;
polycarbonate resin 2: number average molecular weight 23000, S-3000F, mitsubishi;
polycarbonate resin 3: number average molecular weight 16000, H-4000F, mitsubishi;
optical function 1: titanium dioxide R103, duPont;
optical function 2: zinc sulfide, salsa Ha Liben;
optical function 3: zinc oxide, znO-X1, yellow river zinc product;
acid treatment agent 1: oxidized polyethylene grafted maleic anhydride, acid value of 60mgKOH/g,1105A, three wells in Japan;
acid treating agent 2: oxidized polyethylene wax with an acid value of 26mgKOH/g, A-C325, horniweil;
acid treating agent 3: ethylene-acrylic acid copolymer having an acid value of 40mgKOH/g, A-C540A, honiweil;
antioxidant 1: tris (2, 4-di-t-butylphenyl) phosphite, antioxidant 168, basf;
antioxidant 2: bis (2, 6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphate, PEP-36, ai Dike;
antioxidant 3: beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-stearyl alcohol ester, antioxidant 1076 and Basoff.
Preparation methods of examples and comparative examples:
adding the components into a high-speed mixer according to the mixture ratio of table 1/table 2/table 3, and uniformly mixing to obtain a premix; then, putting the obtained premix into a double-screw extruder for melt mixing, extruding and granulating to prepare a polycarbonate composition; wherein the length-diameter ratio of the double-screw extruder is 48:1; the temperature of the twin-screw extruder is set to 230-280 ℃ in the first section of barrel, 240-290 ℃ in the second section of barrel, 240-300 ℃ in the third section of barrel, 240-300 ℃ in the fourth section of barrel, 240-300 ℃ in the fifth section of barrel, 240-300 ℃ in the sixth section of barrel, 240-300 ℃ in the seventh section of barrel, 240-300 ℃ in the eighth section of barrel, 240-300 ℃ in the ninth section of barrel, and 240-300 ℃ in the tenth section of barrel.
The performance testing method comprises the following steps:
(1) Light transmittance: the light transmittance at 550nm and 850nm, respectively, was measured at a thickness of 1.5mm according to the standard GB2810-1981 test equipment PerkinElmer LAMBDA 1050.
(2) Notched Izod impact Strength: the notched Izod impact strength of the untreated sample and the sample after 10min of heat retention at 320℃were measured according to the standard ASTM D256-2010 test, respectively, and calculated: the retention of impact strength after heat treatment of the sample = (notched impact strength of cantilever after heat retention at 320 ℃ for 10 min/notched impact strength of cantilever without heat treatment) ×100%.
Table 1: examples 1 to 7 the proportions of the components (in weight%) and the results of the performance tests
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| PolycarbonatesResin 1 | 99.4 | 99.1 | 98.8 | 98.4 | 98.1 | 98.4 | 98.4 |
| Polycarbonate resin 2 | |||||||
| Optical functional object 1 | 0.2 | 0.5 | 0.8 | 1.2 | 1.5 | ||
| Optical functional object 2 | 1.2 | ||||||
| Optical functional object 3 | 1.2 | ||||||
| Acidic treating agent 1 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Antioxidant 1 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| 550nm light transmittance/% | 14.5 | 13.0 | 10.9 | 8.6 | 8.4 | 7.4 | 8.0 |
| 850nm light transmittance/% | 33.5 | 32.2 | 30.1 | 28.6 | 27.8 | 28.8 | 27.8 |
| Notched impact strength of cantilever beam, J/m | 865 | 836 | 812 | 806 | 795 | 762 | 742 |
| Izod notched impact strength, J/m after 10min heat retention at 320 DEG C | 848 | 821 | 802 | 794 | 774 | 710 | 674 |
| Retention of notched impact strength of cantilever beam% | 98.03 | 98.21 | 98.77 | 98.51 | 97.36 | 93.17 | 90.84 |
Examples 6/7 compared with example 4, the addition of zinc sulfide or zinc oxide has a greater effect on the impact strength and high thermal stability of the material, preferably titanium dioxide is an optical function.
Table 2: examples 8-13 composition (in weight percent) and results of Performance testing
| Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Implementation of the embodimentsExample 13 | |
| Polycarbonate resin 1 | 98.4 | 98.4 | 98.0 | 98.4 | 98.2 | |
| Polycarbonate resin 2 | 98.4 | |||||
| Optical functional object 1 | 1.2 | 1.2 | 1.2 | 1.2 | 1.2 | 1.0 |
| Acidic treating agent 1 | 0.2 | 0.2 | 0.2 | 0.4 | ||
| Acidic treating agent 2 | 0.2 | |||||
| Acidic treating agent 3 | 0.2 | |||||
| Antioxidant 1 | 0.2 | 0.2 | 0.2 | 0.6 | 0.4 | |
| Antioxidant 2 | 0.2 | |||||
| 550nm light transmittance | 8.4 | 7.8 | 7.6 | 8.5 | 7.8 | 9.0 |
| Light transmittance at 850nm | 27.8 | 28.1 | 27.7 | 28.8 | 28.0 | 30.1 |
| Notched impact strength of cantilever beam, J/m | 725 | 785 | 778 | 825 | 802 | 820 |
| Izod notched impact strength, J/m after 10min heat retention at 320 DEG C | 657 | 758 | 749 | 814 | 788 | 808 |
| Retention of notched impact strength of cantilever beam% | 90.62 | 96.56 | 96.27 | 98.66 | 98.25 | 98.54 |
Examples 9/10 are superior to example 4 in that the material added with oxidized polyethylene-grafted maleic anhydride has impact properties and high thermal stability, and oxidized polyethylene-grafted maleic anhydride is preferable as an acidic treating agent.
Table 3: comparative examples 1 to 7 the proportions of the respective components (in weight%) and the results of the respective performance tests
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
| Polycarbonate resin 1 | 97.6 | 99.6 | 98.3 | 98.3 | 97.3 | 98.1 | |
| Polycarbonate resin 3 | 98.1 | ||||||
| Optical functional object 1 | 2.0 | / | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
| Acidic treating agent 1 | 0.2 | 0.2 | / | 0.2 | 0.2 | 0.2 | 0.2 |
| Antioxidant 1 | 0.2 | 0.2 | 0.2 | / | 1.0 | 0.2 | |
| Antioxidant 3 | 0.2 | ||||||
| 550nm light transmittance | 7.6 | 89.1 | 7.8 | 9.0 | 7.2 | 11.8 | 8.2 |
| Light transmittance at 850nm | 24.5 | 89.0 | 26.2 | 27.5 | 24.5 | 30.1 | 28.8 |
| Notched impact strength of cantilever beam, J/m | 785 | 881 | 752 | 748 | 816 | 782 | 586 |
| Izod notched impact strength, J/m after 10min heat retention at 320 DEG C | 741 | 825 | 598 | 605 | 785 | 552 | 322 |
| Retention of notched impact strength of cantilever beam% | 94.39 | 93.64 | 79.52 | 80.88 | 96.20 | 70.59 | 54.95 |
As can be seen from the above examples and comparative examples, the polycarbonate composition prepared by adding a certain amount of optical functional substances, an acidic treating agent and an antioxidant and performing synergistic action of the components has special optical properties of selective infrared transmission (the infrared light transmittance at 850nm with the thickness of 1.5mm is higher than 27% and the visible light transmittance at 550nm is lower than 15%), and can maintain high thermal stability, and the material can still maintain high toughness (the notched Izod impact strength of > 650J/m) after heat treatment at 320 ℃ for 10 min.
Claims (8)
1. A polycarbonate composition, comprising the following components in weight percent:
97.2% -99.7% of polycarbonate resin;
0.1% -1.5% of optical functional substance;
0.1% -0.5% of an acidic treating agent;
0.1% -0.8% of antioxidant;
the number average molecular weight of the polycarbonate resin is 18000-40000;
the optical functional object is selected from any one or more of titanium dioxide, zinc sulfide, zinc oxide or magnesium oxide;
the acid treating agent is selected from any one or more of oxidized polyethylene grafted maleic anhydride, oxidized polyethylene wax or ethylene-acrylic acid copolymer;
the antioxidant is selected from any one or more of bis (2, 6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphate or tri (2, 4-di-tert-butylphenyl) phosphite.
2. The polycarbonate composition of claim 1, comprising the following components in weight percent:
97.8% -99.0% of polycarbonate resin;
0.6% -1.2% of optical functional substance;
0.2% -0.4% of an acidic treating agent;
0.2 to 0.6 percent of antioxidant.
3. The polycarbonate composition of claim 1, wherein the polycarbonate resin has a number average molecular weight of 25000 to 38000.
4. The polycarbonate composition of claim 1, wherein the optical function is titanium dioxide.
5. The polycarbonate composition of claim 1, wherein the acidic treatment agent is selected from the group consisting of oxidized polyethylene grafted maleic anhydride.
6. The polycarbonate composition according to claim 1, wherein the acid value of the acid treatment agent is 20 to 60mgKOH/g.
7. The method for producing a polycarbonate composition according to any one of claims 1 to 6, comprising the steps of: adding the components into a high-speed mixer according to the proportion, and uniformly mixing to obtain a premix; then, putting the obtained premix into a double-screw extruder for melt mixing, extruding and granulating to prepare a polycarbonate composition; wherein the length-diameter ratio of the double-screw extruder is 40:1-48:1; the temperature of the twin-screw extruder was set at 230-300 ℃.
8. Use of the polycarbonate composition of any of claims 1-6 in an indicator light, a remote control, or a wearable device.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090059060A (en) * | 2007-12-05 | 2009-06-10 | 주식회사 엘지화학 | Non-halogen flame retardant polycarbonate resin compound having improved infrared transmissivity |
| KR101838171B1 (en) * | 2016-09-27 | 2018-03-14 | (주)동신폴리켐 | Thermal barrier transparency sheet and manufacturing method thereof |
| CN112724630A (en) * | 2020-12-15 | 2021-04-30 | 金发科技股份有限公司 | Infrared-transmitting flame-retardant polycarbonate composition and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090059060A (en) * | 2007-12-05 | 2009-06-10 | 주식회사 엘지화학 | Non-halogen flame retardant polycarbonate resin compound having improved infrared transmissivity |
| KR101838171B1 (en) * | 2016-09-27 | 2018-03-14 | (주)동신폴리켐 | Thermal barrier transparency sheet and manufacturing method thereof |
| CN112724630A (en) * | 2020-12-15 | 2021-04-30 | 金发科技股份有限公司 | Infrared-transmitting flame-retardant polycarbonate composition and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 透明有机无机复合材料的制备及其光学性能的研究;周奕杰;中国博士学位论文全文数据库 (工程科技Ⅰ辑);B020-31 * |
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