CN101704995B - Polycarbonate blend with low stress optical coefficient - Google Patents
Polycarbonate blend with low stress optical coefficient Download PDFInfo
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Abstract
The invention belongs to the field of polymer materials, relating to a polycarbonate blend with a low stress optical coefficient. The components of the polycarbonate blend comprise bisphenol A polycarbonate and at least one polyester polymer containing a cycloaliphatic ring, such as poly(1,4-cyclohexanedicarboxylicacid-1,4-cyclohexylene dimethylene), polycarbonate containing the cycloaliphatic ring and the like. The blend has a stress optical coefficient lower than that of the bisphenol A polycarbonate while keeping the high transparency and is suitable for plastic parts with low double refraction and high optical quality, such as optical products in the field of aerospace, automobile windows and lamps, optical lenses and lens, compact disks and the like.
Description
Technical field
The invention belongs to polymeric material field, relate to a kind of polycarbonate Alloys with low stress optical coefficient.
Background technology
Bisphenol A polycarbonate (bisphenol A polycarbonate, BPA-PC) because of high transmission rate, high impact properties, good temperature tolerance and excellent creep resistance, become one of most important optically transparent material, it just uses from the ordinary optical field such as optical mirror slip, camera lens, lens etc., gradually to high-end optical field penetrations such as Aeronautics and Astronautics, automobile and photoelectricity, to substitute traditional synthetic glass and unorganic glass.But the high-performance Transparent Parts of aerospace field, require the optical texture and the performance of transparent material even, traditional synthetic glass stress optical coefficient is extremely low, can satisfy this requirement, and the stress optical coefficient of bisphenol A polycarbonate reaches 80 Brewsters (1Brewster=1 * 10
-121/Pa), exceed more than 10 times, very easily produce the ununiformity of optical property than synthetic glass; CD for photoelectric field, its disk substrate material must have low-birefringence, because the double refraction meeting causes the polarization laser that scans and write can not vernier focusing, cause CD write with reproduction process in introduce problem such as noise, the low-birefringence of optical goods requires its material must have low stress optical coefficient, and the stress optical coefficient height of bisphenol A polycarbonate is difficult to meet the demands.
The stress optical coefficient of so-called material, it is a kind of parameter of representing the internal stress of these forming materials goods to the optical property influence degree, be the inherent feature parameter of material, the relation of the stress optical coefficient C of material and the birefringence n of moulded products and internal stress Δ σ is as follows:
Δn＝C×Δσ (1)
C is the stress optical coefficient of material in the formula (1), and Δ σ is the internal stress of product.For polymkeric substance, the macromolecular orientation of internal stress during with forming process is relevant, and its essence is that high elastic deformation is frozen in the goods and forms, and can drop to minimum by process optimization; But stress optical coefficient is a kind of the constant relevant with material itself.Stress optical coefficient is low more, and double refraction is just more little.Desire obtains low-birefringence, high optical quality goods, selects for use the low stress optical coefficient material just to seem very important.
Adopt lower polymkeric substance and the bisphenol A polycarbonate of stress optical coefficient to carry out blending and modifying, it is a kind of important method that obtains the low stress optical coefficient material, but obtain high transparent blends, one of them cardinal principle is almost completely consistent or both materials of the specific refractory power between the requirement blend components can mix fully (being that molecular level mixes).Can mix and have the polymkeric substance of low stress optical coefficient fully with bisphenol A polycarbonate, be rarely found.
Summary of the invention
The objective of the invention is to propose a kind of transparent polycarbonate blend with low stress optical coefficient with low stress optical coefficient.Technical scheme of the present invention is that the chemical composition of this blend is:
(a) bisphenol A polycarbonate;
(b) poly-(1,4 cyclohexanedicarboxylic acid-1,4 cyclohexanedimethanoester ester);
(c) aromatic copolycarbonate of fatty ring
Wherein get 30～80 parts of bisphenol A polycarbonates by weight, poly-(1,4-cyclohexane cyclohexanedimethanodibasic-1,4 cyclohexanedimethanoester esters) and the parts by weight sum of the aromatic copolycarbonate of fatty ring be 70～20 parts, wherein gather (1,4-cyclohexane cyclohexanedimethanodibasic-1,4 cyclohexanedimethanoester ester) and the aromatic copolycarbonate weight ratio between the two of fatty ring from 100: 0 to 0: 100.
Described bisphenol A polycarbonate has following structural unit:
Described poly-(1,4 cyclohexanedicarboxylic acid-1,4 cyclohexanedimethanoester ester) has following structural unit:
The aromatic copolycarbonate of described fatty ring has following structural unit:
R in the formula
1, R
2And R
3All are alkyl, and have at least an alkyl to contain cycloaliphatic ring, m and n are 0～4 integers, and p is 1～12 integer.
The aromatic copolycarbonate of described fatty ring comprises based on 1, two (the 4-hydroxy phenyls)-3,3 of 1-', the polycarbonate of 5-trimethyl-cyclohexane (TMC-PC) has following structural unit:
The typical unit of structure III includes but not limited to 1 except that TMC-PC, two (4-the hydroxy phenyl)-hexanaphthenes (BBC), 1 of 1-, and two (4-the hydroxy phenyl)-pentamethylene and 3,3 of 1-'-the dicyclohexyl bis-phenol.
The stress optical coefficient of bisphenol A polycarbonate is high excessive relevant with the polarity difference of its macromolecular chain different directions.Contain the polyester polymer (comprising polycarbonate) of cycloaliphatic ring in some macromolecular chains, stress optical coefficient is on the low side, and optical property more trends towards isotropy.This may be the introducing owing to cycloaliphatic ring, helps reducing the difference of macromolecular chain main chain direction and side chain direction polarization rate.
Advantage that the present invention has and beneficial effect promptly are cycloaliphatic ring polyester polymer and the bisphenol A polycarbonate blend with stress optical coefficient, thereby obtain polycarbonate blend with low stress optical coefficient.
Poly-(1,4 cyclohexanedicarboxylic acid-1, the 4 cyclohexanedimethanoester ester) stress optical coefficient (PCCD) of present cycloaliphatic polyesters is 30 Brewsters, far below bisphenol A polycarbonate.Experiment shows, the BPA-PC/PCCD blend of the different proportionings of preparing by melt-blending process all is transparent.The employing differential scanning calorimetry detects, and blend all only shows single glass transition temperature (Tg), and this explanation PCCD and BPA-PC can mix fully.Adopt PCCD and BPA-PC blend, can obtain transparent blends than low stress optical coefficient.The Tg of PCCD (60 ℃) is more much lower than BPA-PC, therefore adopts PCCD and BPA-PC blend, can also improve the moulding processability of BPA-PC, if but add too much PCCD, can obviously reduce the resistance to elevated temperatures of blend.
The aromatic copolycarbonate of some fatty rings also has lower stress optical coefficient, stress optical coefficient as TMC-PC is 38 Brewsters, can mix fully with BPA-PC, therefore adopt TMC-PC and BPA-PC blend, can obtain transparent blends than low stress optical coefficient.The Tg of TMC-PC (reaching 238 ℃) adopts TMC-PC and BPA-PC blend than BPA-PC height in addition, can also improve resistance to elevated temperatures, but the high Tg of TMC-PC causes the moulding processability difficulty, and notched Izod impact strength is also low than BPA-PC simultaneously.
The BPA-PC/PCCD/TMC-PC blend that PCCD, TMC-PC and BPA-PC blend is simultaneously prepared has lower stress optical coefficient equally, and can take into account the requirement of others such as moulding processability, resistance to elevated temperatures and impelling strength better.
Can adopt phosgenation or ester-interchange method to synthesize BPA-PC used among the present invention.For TMC-PC,, adopt the phosgene interface polycondensation, easier acquisition high-molecular weight polycarbonate because steric effect is bigger.BPA-PC that adopts among the present invention and TMC-PC, preferred number-average molecular weight (Mn) is about 10,000～100,000, and more preferably from about 12,000～38,000.
Can synthesize used PCCD in the invention by alcoholic acid esterification method or pure ester-interchange method.The alcoholic acid esterification method is to adopt 1,4-cyclohexanedimethanol and 1, the 4-cyclohexane cyclohexanedimethanodibasic carries out melt polycondensation reaction preparation and comes in the presence of a kind of catalyzer, the alcohol ester-interchange method is to adopt 1,4-cyclohexanedimethanol and 1,4-hexanaphthene dimethyl ester carry out the preparation of first transesterify aftercondensated and come under the condition of transesterification catalyst, the number-average molecular weight (Mn) of preferred PCCD reaches 20, more than 000, second-order transition temperature reaches more than 60 ℃.
Preparation method with polycarbonate Alloys of low stress optical coefficient of the present invention includes but not limited to melt-blending process, solution method and coetrusion etc.Wherein preferential method is a melt-blending process.
The step of melt-blending process is at first to carry out premix by the aromatic copolycarbonate of filling a prescription polycarbonate, poly-(1,4 cyclohexanedicarboxylic acid-1,4 cyclohexanedimethanoester ester) and fatty ring on high-speed mixer; Carry out drying and dehydrating then, dehydration can be carried out in 40～120 ℃ vacuum drying oven or baking oven, after the time is 6～12hr; Adopt twin screw extruder or Banbury mixer to carry out melt blending the Preblend behind the drying and dehydrating, the blending temperature scope is 220～300 ℃, and screw speed is 160～250r/min.
Embodiment
Below with reference to embodiment technical solution of the present invention is further described.
Embodiment 1～6
Bisphenol A polycarbonate (BPA-PC), poly-(1,4 cyclohexanedicarboxylic acid-1,4 cyclohexanedimethanoester ester) (PCCD) are required to weigh according to the prescription in the table 1, and the gross weight of each embodiment is measured 1000g.After mixing on the high-speed mixer, to put vacuum drying oven into and carry out drying treatment, the loft drier internal pressure is less than 1000Pa, and drying temperature is 40～60 ℃, and be 6～12 hours time of drying.The dry first batch mixing of crossing is gone up melt blending at twin screw extruder (Werner Pleiderer company, model is ZSK-25WLE), and blending temperature is 220～270 ℃, and screw speed is 160～250r/min, and cooling granulation obtains the blend pellet then.
Table 1
| BPA-PC/％ | PCCD/％ | |
| Comparative Examples 1 | 100 | |
| Comparative Examples 2 | 100 | |
| Embodiment 1 | 80 | 20 |
| Embodiment 2 | 70 | 30 |
| Embodiment 3 | 60 | 40 |
| Embodiment 4 | 50 | 50 |
| Embodiment 5 | 40 | 60 |
| Embodiment 6 | 30 | 70 |
Require the blend pellet is carried out injection moulding on injection moulding machine according to corresponding standard, prepare the performance test batten, carry out performance test again, wherein second-order transition temperature adopts differential scanning calorimeter (U.S. Perkin Elmer company, DSC-7) test, transparence adopts transmittance/mist degree tester (Shanghai Precision Scientific Apparatus Co., Ltd, WGT-S) test, stress optical coefficient adopts the test of run-in index photoelastic equipment, notched Izod impact strength adopts tension testing machine (American I NSTRON company, 4466) melt flow index instrument (scientific instrument factory of Jilin University, XRZ-400) test are adopted in test, melt flow rate (MFR).Test result is as shown in table 2.
Table 2
| Second-order transition temperature/℃ | Transparence/% | Stress optical coefficient/Brewsters | Notched Izod impact strength/kJ/m 2 | Melt flow rate (MFR)/g/10min (300 ℃) | |
| Comparative Examples 1 | 151.5 | 89.5 | 80 | 70 | ?5.8 |
| Comparative Examples 2 | 60.4 | 90.2 | 30 | 55 | ?-- |
| Embodiment 1 | 115.1 | 88.8 | 68 | 63 | ?12.5 |
| Embodiment 2 | 102.5 | 88.4 | 66 | 62 | ?13.8 |
| Embodiment 3 | 92.7 | 88.6 | 61 | 63 | ?16.3 |
| Embodiment 4 | 85.9 | 88.2 | 58 | 59 | ?20.6 |
| Embodiment 5 | 78.2 | 87.3 | 52 | 57 | ?22.3 |
| Embodiment 6 | 75.0 | 86.7 | 44 | 56 | ?25.9 |
As can be seen from Table 2, (BPA-PC) compares with bisphenol A polycarbonate, and poly-(1,4 cyclohexanedicarboxylic acid-1,4 cyclohexanedimethanoester ester) be stress optical coefficient low (be BPA-PC 37.5%) (PCCD), but second-order transition temperature too low (60.4 ℃).After the BPA-PC blend: the polycarbonate Alloys of different proportionings all has only a second-order transition temperature, and all has the good transparency, illustrates that BPA-PC and PCCD are fully compatible; Stress optical coefficient all is lower than BPA-PC, and along with the increase of PCCD content, stress optical coefficient constantly reduces; Second-order transition temperature (〉=75 ℃) is higher than pure PCCD, and compares with BPA-PC, and melt flow rate (MFR) obviously increases, and shows that processing characteristics is improved, and has higher notched Izod impact strength simultaneously.
Compare with bisphenol A polycarbonate, the characteristics of blend are stress optical coefficient lower (less than 70 Brewsters) in the table 1, and plastic performance is better.
Embodiment 7～12
With bisphenol A polycarbonate (BPA-PC) with based on 1, two (the 4-hydroxy phenyls)-3,3 of 1-', the polycarbonate of 5-trimethyl-cyclohexane (TMC-PC) requires to weigh according to the prescription in the table 3, and the gross weight of each embodiment is measured 1000g.After mixing on the high-speed mixer, to put baking oven or vacuum drying oven into and carry out processed, drying temperature is 80～120 ℃, be 6～12 hours time of drying.The dry first batch mixing of crossing is gone up melt blending at twin screw extruder (Werner Pleiderer company, model is ZSK-25WLE), and blending temperature is 250～300 ℃, and screw speed is 160～250r/min, and cooling granulation obtains the blend pellet then.Test result sees Table 3.
Table 3
| BPA-PC/％ | TMC-PC/％ | |
| Comparative Examples 3 | 100 | |
| Embodiment 7 | 80 | 20 |
| Embodiment 8 | 70 | 30 |
| Embodiment 9 | 60 | 40 |
| Embodiment 10 | 50 | 50 |
| Embodiment 11 | 40 | 60 |
| Embodiment 12 | 30 | 70 |
As can be seen from Table 4, compare with BPA-PC, TMC-PC stress optical coefficient low (be BPA-PC 47.5%), but second-order transition temperature too high (238.2 ℃), formability is poor, and notched Izod impact strength is low simultaneously.After the BPA-PC blend: the polycarbonate Alloys of different proportionings all has only a second-order transition temperature, and all has the good transparency, illustrates that BPA-PC and TMC-PC are fully compatible; Stress optical coefficient all is lower than BPA-PC; Second-order transition temperature is higher 10～50 ℃ than BPA-PC.
Compare with bisphenol A polycarbonate, the characteristics of blend are stress optical coefficient lower (≤70 Brewsters) in the table 3, and resistance to elevated temperatures is better.
Table 4
| Second-order transition temperature/℃ | Transparence/% | Stress optical coefficient/Brewsters | |
| Comparative Examples 1 | 151.5 | 89.5 | 80 |
| Comparative Examples 3 | 238.2 | 88.5 | 38 |
| Embodiment 7 | 161.6 | 88.6 | 70 |
| Embodiment 8 | 170.1 | 87.8 | 67 |
| Embodiment 9 | 175.4 | 87.4 | 64 |
| Embodiment 10 | 186.6 | 87.1 | 60 |
| Embodiment 11 | 190.2 | 86.5 | 55 |
| Embodiment 12 | 200.2 | 86.3 | 49 |
Embodiment 13～19
Adopt embodiment 7～12 described methods, difference is to have added among the embodiment PCCD.Concrete proportioning and test result are respectively shown in table 5 and table 6.
Embodiment 1～12 explanation, polycarbonate Alloys BPA-PC/PCCD and BPA-PC/TMCPC all have lower stress optical coefficient (≤70 Brewsters), but the Tg of BPA-PC/PCCD is starkly lower than BPA-PC in the table 2, and resistance to elevated temperatures reduces, and plastic performance is better; And the Tg of BPA-PCPC/TMCPC is apparently higher than BPA-PC in the table 4, and resistance to elevated temperatures is better, and plastic performance reduces.
Blend BPA-PC/PCCD/TMCPC in the table 5 more lays particular stress on over-all properties, the BPA-PC content of embodiment 13～19 is identical, but the relative content of PCCD and TMC-PC is different, table 6 shows that the stress optical coefficient of blend is basic identical, but compare with embodiment 8 (BPA-PC/TMC-PC=70/30) in the table 3 with embodiment 2 (BPA-PC/PCCD=70/30) in the table 1, the second-order transition temperature of blend can be regulated in wideer scope, even can be consistent with the second-order transition temperature of pure bisphenol A polycarbonate, can satisfy under the condition of low stress optical coefficient so in practice, require and the formability requirement according to heatproof, further regulate the prescription of blend component, thereby widened range of application.
Table 5
| BPA-PC/％ | PCCD/％ | TMC-PC/％ | |
| Embodiment 13 | 70 | 25 | 5 |
| Embodiment 14 | 70 | 20 | 10 |
| Embodiment 15 | 70 | 15 | 15 |
| Embodiment 16 | 70 | 10 | 20 |
| Embodiment 17 | 70 | 8 | 22 |
| Embodiment 18 | 70 | 7 | 23 |
| Embodiment 19 | 70 | 5 | 25 |
Table 6
| Second-order transition temperature/℃ | Transparence/% | Stress optical coefficient/Brewsters | |
| Embodiment 13 | 111.4 | 88.5 | 65.4 |
| Embodiment 14 | 119.7 | 88.3 | 65.8 |
| Embodiment 15 | 129.3 | 88.0 | 66.2 |
| Embodiment 16 | 140.5 | 88.1 | 66.6 |
| Embodiment 17 | 145.5 | 87.8 | 66.8 |
| Embodiment 18 | 148.3 | 87.8 | 66.9 |
| Embodiment 19 | 153.9 | 87.6 | 67 |
More than the described polycarbonate Alloys of each embodiment, compare with bisphenol A polycarbonate, all have lower stress optical coefficient, can be applicable to the transparent plastic article of different occasions.During practical application, only otherwise leave the spirit and scope of the present invention, obviously can be according to the specific requirement of aspects such as stress optical coefficient, formability, resistance to elevated temperatures and mechanical property, change or revise.
Claims (1)
1. polycarbonate Alloys with low stress optical coefficient, the component of this blend comprises:
(a) bisphenol-a polycarbonate;
(b) poly-(1,4 cyclohexanedicarboxylic acid-1,4 cyclohexanedimethanoester ester);
(c) aromatic copolycarbonate of fatty ring,
Described blend adopts following method preparation: with bisphenol A polycarbonate (BPA-PC), based on 1, and two (the 4-hydroxy phenyls)-3,3 of 1-', the polycarbonate of 5-trimethyl-cyclohexane (TMC-PC) and poly-(1,4-cyclohexane cyclohexanedimethanodibasic-1,4 cyclohexanedimethanoester ester) set of dispense ratio (PCCD) is selected from BPA-PC/%: PCCD/%: TMC-PC/% was respectively 70: 25: 5,70: 20: 10,70: 15: 15,70: 10: 20,70: 8: 22,70: 7: 23,70: 5: 25; Gross weight is measured 1000g; After mixing on the high-speed mixer, to put baking oven or vacuum drying oven into and carry out processed, drying temperature is 80～120 ℃, be 6～12 hours time of drying; The dry first batch mixing of crossing is in twin screw extruder Werner Pleiderer company, and model is that ZSK-25WLE goes up melt blending, and blending temperature is 250～300 ℃, and screw speed is 160～250r/min, and cooling granulation obtains the blend pellet then.
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| WO2013120269A1 (en) * | 2012-02-17 | 2013-08-22 | Sabic Innovative Plastics Ip B.V. | Transparent thin-wall scratch-resistant article |
| CN106832142B (en) * | 2016-12-27 | 2019-05-03 | 天津金发新材料有限公司 | A kind of filling PC composition |
| CN106810840B (en) * | 2016-12-27 | 2019-05-10 | 天津金发新材料有限公司 | A kind of novel low stress PC composition |
| CN113929894B (en) * | 2021-11-30 | 2024-01-30 | 万华化学集团股份有限公司 | High-temperature-resistant polycarbonate copolymer and preparation method and application thereof |
| CN114230776B (en) * | 2021-12-28 | 2023-04-11 | 丹阳市正阳光学有限公司 | Method for processing multifocal spectacle lens |
| CN115466477A (en) * | 2022-09-13 | 2022-12-13 | Oppo广东移动通信有限公司 | Optical material, preparation method, lens, camera module and electronic equipment |
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| CN101120033A (en) * | 2004-12-22 | 2008-02-06 | 拜尔材料科学股份公司 | Polycarbonate substrate material for transparent injection-molded parts |
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