CN116102861A - Light aging-resistant brominated flame-retardant PC/PBT alloy composition, and preparation method and application thereof - Google Patents
Light aging-resistant brominated flame-retardant PC/PBT alloy composition, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a light aging resistant brominated flame-retardant PC/PBT alloy composition, and a preparation method and application thereof. The photoaging-resistant brominated flame-retardant PC/PBT alloy composition comprises the following components in parts by weight: 30-65 parts of PC, 15-30 parts of brominated PC, 18-40 parts of PBT, 3-10 parts of toughening agent, 0.5-5 parts of antimony white, 0.1-0.8 part of transesterification inhibitor, 0.1-1 part of weather-proof agent and 0.2-2 parts of anti-dripping agent. The brominated flame-retardant PC/PBT alloy composition has good flame retardant property and impact strength, and can still maintain good flame retardant property and impact strength after photo-aging.
Description
Technical Field
The invention relates to the field of engineering plastics, in particular to a light aging resistant brominated flame-retardant PC/PBT alloy composition, and a preparation method and application thereof.
Background
The brominated flame-retardant polycarbonate/polybutylene terephthalate (PC/PBT) alloy is a high-performance alloy material, has the advantages of low internal stress, high toughness, high surface glossiness, good processing fluidity and the like, and meanwhile, the chemical resistance of the alloy material can be obviously improved by adding the polybutylene terephthalate, so that the application field of the alloy material is further expanded, and the alloy material is widely applied to the fields of electronic appliances, kitchens and bathrooms, audio-visual equipment, low-speed travel and the like.
In the prior art, brominated flame retardants commonly selected for brominated flame-retardant PC/PBT alloys include brominated polycarbonate, brominated epoxy, brominated polystyrene and the like, such as Chinese patent names halogen-free sulfonate and/or sulfinate used as flame retardants, flame retardant synergists and free radical generators in plastics, and the brominated flame retardants can bring about better flame retardant effect. However, the required brominated flame retardant in the brominated flame-retardant PC/PBT alloy has higher addition, which greatly influences the mechanical properties of the alloy material, in particular the impact strength; in addition, the brominated flame retardant is easy to degrade in the photo-aging process, so that the flame retardant property of the alloy material after photo-aging can be obviously reduced, and the impact strength of the alloy material after photo-aging can be obviously reduced, and the brominated flame retardant PC/PBT alloy is obviously limited in an outdoor application environment.
Therefore, the problems that the impact strength of the existing brominated flame-retardant PC/PBT alloy is not high, and the flame retardant property and the impact strength are obviously reduced after photo-aging are solved.
Disclosure of Invention
The primary purpose of the invention is to overcome the problems that the impact strength of the prior brominated flame-retardant PC/PBT alloy is not high and the flame retardant property and the impact strength are obviously reduced after photo-aging, and provide a brominated flame-retardant PC/PBT alloy composition resistant to photo-aging. The brominated flame-retardant PC/PBT alloy composition has good flame retardant property and impact strength, and can still maintain good flame retardant property and impact strength after photo-aging.
The invention further aims to provide a preparation method of the brominated flame-retardant PC/PBT alloy composition.
The invention further aims to provide application of the brominated flame-retardant PC/PBT alloy composition in preparing low-speed travel equipment products.
The above object of the present invention is achieved by the following technical solutions:
the light aging resistant brominated flame-retardant PC/PBT alloy composition comprises the following components in parts by weight:
the brominated PC is phosgene, tetrabromobisphenol A and a copolymer of bisphenol A; the initial decomposition temperature of the brominated PC is more than or equal to 460 ℃; the ratio of the sum of the masses of PC and brominated PC to the mass of PBT is 1: (0.2-0.7).
It should be understood that the initial decomposition temperature of the present invention refers to: the initial decomposition temperature is obtained by recording the temperature of 5% of the mass loss of the measured object (such as brominated PC) from room temperature to 750 ℃ at a heating rate of 20 ℃/min under nitrogen atmosphere by a thermal weight loss analysis Tester (TGA).
The inventor of the invention unexpectedly discovers that the brominated PC with specific initial decomposition temperature is added, and the mass ratio of PC to brominated PC to PBT is controlled within a specific range, so that the brominated flame-retardant PC/PBT alloy composition has good flame retardant property and impact strength, and the flame retardant property and impact strength after photo aging are kept good. The reason for this is: when the mass ratio of PC to brominated PC to PBT is controlled within a specific range, the material can form a uniform and stable sea-island morphology structure which takes PC and brominated PC as continuous phases and PBT as sea-island phases, and the sea-island morphology structure can enable the initial impact strength of the material to reach a higher level on the one hand; on the other hand, the island-shaped morphology structure ensures that the phase state and phase interface of the material are stable in the photo-aging process, brominated PC is not obviously degraded in the photo-aging process to generate micromolecular substances, and the obtained brominated flame-retardant PC/PBT alloy composition can still maintain good flame retardant property and impact strength after photo-aging through the synergistic effect of the island-shaped morphology structure and the brominated PC with specific initial decomposition temperature.
Namely, the brominated flame-retardant PC/PBT alloy composition has good flame retardant property and impact strength, and can still maintain good flame retardant property and impact strength after photo-aging.
Preferably, the brominated flame-retardant PC/PBT alloy composition comprises the following components in parts by weight:
preferably, the brominated PC has an initial decomposition temperature of 466 to 489 ℃.
Preferably, the mass fraction of bromine element in the brominated PC is 20-22%.
The synthesis of brominated PCs of the present invention can be referred to conventional process steps for the synthesis of polycarbonates.
The invention provides a better preparation method for synthesizing brominated PC, in particular to a preparation method for synthesizing brominated PC:
the preparation method of the brominated PC comprises the following steps: bisphenol A, tetrabromobisphenol A, 8-12% sodium hydroxide aqueous solution and sodium bisulphite are mixed and stirred for 1-2 hours at 20-30 ℃ to generate bisphenol A and tetrabromobisphenol A sodium salt; adding methylene dichloride solution containing 8-12% of phosgene, cooling to-3 ℃, and continuously stirring to perform interfacial polycondensation reaction; and standing for 1-2 hours, removing supernatant, washing the lower turbid liquid to be neutral by deionized water, precipitating the product by absolute ethyl alcohol, filtering and drying to obtain the brominated PC.
Wherein, brominated PC with different initial decomposition temperatures can be obtained by regulating and controlling the interfacial polycondensation reaction time and the dosage of phosgene concentration; by regulating the dosage ratio of bisphenol A and tetrabromobisphenol A, brominated PC with different mass fractions of bromine elements can be obtained.
PC, PBT, tougheners, transesterification inhibitors, weathering agents and anti-drip agents commonly used in the art can be used in the present invention.
Preferably, the average molecular weight of the PC is 25000 to 36000.
Preferably, the PBT has a viscosity of from 0.85 to 1dl/g.
Preferably, the toughening agent is an acrylic-silicone rubber type toughening agent.
Preferably, the transesterification inhibitor is sodium dihydrogen phosphate.
Optionally, the weathering agent is at least one of 2- (2 ' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole or 2- [ 2-hydroxy-4- [3- (2-ethylhexyloxy) -2-hydroxypropoxy ] phenyl ] -4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazine.
Optionally, the anti-dripping agent is SAN coated PTFE or PTFE pure powder.
Preferably, the brominated flame retardant PC/PBT alloy composition also comprises 0.01-2 parts of processing aid.
More preferably, the processing aid is an antioxidant or lubricant.
Alternatively, the antioxidant is at least one of tetrakis [ methylene (3, 5-di-tert-butyl-4-hydroxyhydrocinnamate) ] methane, tris (2, 4-di-tert-butylphenyl) phosphite or distearylthiopropionate.
Optionally, the lubricant is at least one of pentaerythritol stearate, polyethylene wax, or a silicone lubricant.
The preparation method of the brominated flame-retardant PC/PBT alloy composition comprises the following steps: and mixing the components, melting, extruding and granulating to obtain the brominated flame-retardant PC/PBT alloy composition.
Preferably, the preparation method comprises the following steps: and stirring and mixing the components, then melting in a double-screw extruder, extruding and granulating to obtain the brominated flame-retardant PC/PBT alloy composition.
More preferably, the length-diameter ratio of the double-screw extruder is 40-45:1, the screw barrel temperature is 210-260 ℃, and the screw rotating speed is 500-600 rpm.
The application of the brominated flame-retardant PC/PBT alloy composition in preparing low-speed trip equipment products is also in the protection scope of the invention.
Preferably, the low-speed travel equipment product is a charging pile or a sharing bicycle lock.
Compared with the prior art, the invention has the beneficial effects that:
the brominated flame-retardant PC/PBT alloy composition has good flame retardant property and impact strength, and can still maintain good flame retardant property and impact strength after photo-aging.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples for the purpose of illustration and not limitation, and various modifications may be made within the scope of the present invention as defined by the appended claims.
The reagents selected for the examples and comparative examples of the present invention are described below:
PC1#:1300 10NP, korean LG chemical Co., ltd., average molecular weight 25000;
PC2#:7030PJ, mitsubishi, japan, average molecular weight 36000;
PC3#:7025PJ, mitsubishi group, japan, average molecular weight 28000;
PC4#:1300 22NP, korean LG chemical Co., ltd., average molecular weight 20000;
PBT1#: GX112, china petrochemical instrumentation chemical fiber Limited liability company, viscosity 0.85mL/g;
PBT2#: GX121, china petrochemical industry, chemical industry, inc., with viscosity of 0.98mL/g
PBT3#:1100-211M, manufactured by Taiwan vinca resin Co., ltd., china, with a viscosity of 1.0dl/g;
PBT4#: GL236, china petrochemical industry, chemical fiber, inc., with a viscosity of 1.3dl/g;
toughening agent 1#: acrylic acid-silicon rubber toughening agent, S-2130, mitsubishi Japanese;
toughening agent # 2: methyl methacrylate-butadiene-styrene copolymer, M-521, japan brillouin;
transesterification inhibitor # 1: sodium dihydrogen phosphate, MSP2040, chemical industry;
transesterification inhibitor # 2: zinc dihydrogen phosphate, BUDIT T21, bourdon sea m, germany;
weather-resistant agent: 2- (2 ' -hydroxy-3 ',5' bis (a, a-dimethylbenzyl) phenyl) benzotriazole, commercially available;
anti-drip agent: polytetrafluoroethylene, commercially available;
processing aid: an antioxidant, tetrakis [ methylene (3, 5-di-tert-butyl-4-hydroxyhydrocinnamate) ] methane, commercially available;
antimony white: are commercially available.
Brominated PC1#: the preparation method comprises the following steps: 300g of bisphenol A, 100g of tetrabromobisphenol A, 1800g of 10% sodium hydroxide aqueous solution and 1g of sodium bisulphite are added into a reaction kettle and stirred for 1 hour at 25 ℃ to generate bisphenol A sodium salt and tetrabromobisphenol A sodium salt; 5000g of a 10% phosgene in methylene chloride solution was then added and cooled to 0℃and interfacial polycondensation was carried out with continuous stirring for 1.5h. Standing the reaction kettle for 1 hour, pouring out supernatant, washing the lower turbid liquid to be neutral by deionized water, precipitating the product by 10Kg of absolute ethyl alcohol, filtering, and drying in an oven at 100 ℃ for 12 hours to obtain brominated PC1#. The initial decomposition temperature of the brominated PC1# is 466 ℃, and the bromine content is 22% by adopting an X-ray fluorescence spectrometry.
Brominated PC2#: the self-made preparation method is basically the same as the preparation method of the brominated PC1# and is different in that: 5600g of a 10% phosgene in methylene chloride solution are added; continuous stirring is carried out for interfacial polycondensation for 1.85h. Finally, brominated PC2# is obtained. The initial decomposition temperature of the brominated PC2# is 489 ℃, and the bromine content is 21% by adopting an X-ray fluorescence spectrometry.
Brominated PC3#: the self-made preparation method is basically the same as the preparation method of the brominated PC1# and is different in that: 4700g of a 10% phosgene in methylene chloride solution was added; continuous stirring is carried out for interfacial polycondensation for 1.28h. Finally, brominated PC3# -is obtained. The initial decomposition temperature of the brominated PC3# is 460 ℃, and the bromine content is 22%.
Brominated PC4#: the self-made preparation method is basically the same as the preparation method of the brominated PC1# and is different in that: 335 g bisphenol A and 100g tetrabromobisphenol A. The initial decomposition temperature of brominated PC4# was 466 ℃ and the bromine content was 20% as determined by X-ray fluorescence spectroscopy.
Brominated PC5#: the self-made preparation method is basically the same as the preparation method of the brominated PC1# and is different in that: 420 g of bisphenol A and 100g of tetrabromobisphenol A. The initial decomposition temperature of brominated PC5# was 466 ℃ and the bromine content was 15% as determined by X-ray fluorescence spectroscopy.
Brominated PC6#: the self-made preparation method is basically the same as the preparation method of the brominated PC1# and is different in that: 4500g of a 10% phosgene in methylene chloride solution was added; and continuously stirring to perform interfacial polycondensation reaction for 1h. Finally, brominated PC6# is obtained. The initial decomposition temperature of brominated PC6# is 392 ℃, and the bromine content is 22% by adopting an X-ray fluorescence spectrometry.
Brominated PC7#: the self-made preparation method is basically the same as the preparation method of the brominated PC1# and is different in that: bisphenol A is not added; continuous stirring is carried out for interfacial polycondensation for 1.5h. Finally, brominated PC7# is obtained, the initial decomposition temperature of the brominated PC7# is 460 ℃, and the bromine content is 58% by adopting an X-ray fluorescence spectrometry.
Brominated polycarbon: FG8500, onset decomposition temperature 446 ℃, japanese emperor;
brominated epoxy: f-2100, initial decomposition temperature 364 ℃, israel chemical industry;
brominated polyphenylene: SAYTEX 621, initial decomposition temperature 379 ℃, yabao in U.S.
The components (e.g., weathering agent, anti-drip agent, other adjuvants) selected in each of the parallel examples and comparative examples are the same commercially available products, unless otherwise specified.
The brominated flame-retardant PC/PBT alloy compositions provided by the examples and the comparative examples of the invention have the following performance measured by a test method:
impact strength: the impact strength of the bars was tested according to ASTM D256-2010 standard; in addition, according to ISO 4892.2:2013 standard, ageing test is carried out, the spline is put into a xenon lamp ageing box to carry out xenon lamp ageing, after 1000 hours, the spline is taken out to carry out impact strength test, the result is recorded, the retention rate of impact strength before and after ageing is compared to be used as the judgment of the quality of light ageing resistance stability, and the higher the retention rate of the performance is, the better the ageing stability of the xenon lamp is.
Flame retardant properties: flammability test according to the standard "flammability test of plastics materials, UL 94-2019"; and placing the sample strip into a xenon lamp aging box for xenon lamp aging, taking out the sample strip after 1000 hours for flammability test, and recording the result. Flame retardant rating was derived based on burn rate, extinguishing time, ability to resist dripping, and whether dripping was burning or not, samples for testing: 125mm length and 13mm width, the thickness is 1.0mm when the invention is tested, and the flame retardant grades of the materials can be classified into UL 94V 0, V1, V2 and the like according to UL94-2019 standard.
The preparation process of the brominated flame-retardant PC/PBT alloy composition of each embodiment and the comparative example is as follows: uniformly mixing the components according to a formula to obtain a premix; the premix is put into a double screw extruder, and is melted and mixed in the double screw extruder (the length-diameter ratio of the screw is 45:1, the temperature of a screw cylinder is 250 ℃ and the rotating speed of the screw is 500 rpm) and extruded and granulated, so that the brominated flame-retardant PC/PBT alloy composition is obtained.
Examples 1 to 20
Examples 1-20 provide a series of brominated flame retardant PC/PBT alloy compositions having the formulations shown in tables 1 and 2.
Table 1 formulations (parts by weight) of examples 1 to 8
Table 2 formulations (parts by weight) of examples 9 to 20
Comparative example 1
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 1 in the formulation: the brominated PC1# is replaced by brominated PC6#.
Comparative example 2
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 1 in the formulation: brominated PC1# was replaced with brominated PC7#.
Comparative example 3
This comparative example is a PC/PBT alloy composition having a formulation different from that of example 1 in that: no brominated pc1# was added.
Comparative example 4
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 1 in the formulation: brominated PC1# was replaced with brominated polycarbon.
Comparative example 5
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 1 in the formulation: brominated PC1# was replaced with brominated epoxy.
Comparative example 6
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 1 in the formulation: brominated PC1# was replaced with brominated polystyrene.
Comparative example 7
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 6 in the formulation: the amount of PBT1# was 14 parts, and the mass ratio of (PC+brominated PC) PBT was 1:0.15.
comparative example 8
This comparative example is a brominated flame retardant PC/PBT alloy composition, which differs from example 7 in the formulation: the amount of PBT1# was 40 parts, and the mass ratio of (PC+brominated PC) PBT was 1:0.8.
the properties of the brominated flame retardant PC/PBT alloy compositions/PC/PBT alloy compositions of the examples and comparative examples were measured according to the above-mentioned test methods, and the test results are shown in Table 3.
TABLE 3 results of Performance test of examples and comparative examples
As can be seen from table 3:
the initial flame retardant properties of the brominated flame retardant PC/PBT alloy compositions of examples 1-20 are V-0 level, the initial impact strength is over 669J/m, the flame retardant properties after aging of a xenon lamp are maintained at V-0 level, and the retention rate of the impact strength after aging of the xenon lamp is over 72%, which indicates that the brominated flame retardant PC/PBT alloy composition of the invention has good flame retardant properties and impact strength, and can still maintain good flame retardant properties and impact strength after photo aging.
From examples 1 to 5, it is understood that the retention rate of the impact strength of the obtained brominated flame retardant PC/PBT alloy composition after aging by xenon lamp was 83% or more by controlling the amounts of the respective components within the appropriate ranges (examples 1, 4, 5).
As is clear from examples 1 and 9 to 11, the initial impact strength of the obtained brominated flame-retardant PC/PBT alloy composition was 702J/m or more, and the retention of impact strength after aging with a xenon lamp was 78% or more, using a polycarbonate having an appropriate average molecular weight (25000 to 36000).
As is clear from examples 1 and 12 to 13, the brominated PC having an initial decomposition temperature within a specific range (466 to 489 ℃ C.) was selected, and the obtained brominated flame-retardant PC/PBT alloy composition had a higher initial impact strength (703J/m or more) and a higher retention of impact strength (83% or more) after aging with a xenon lamp.
As is clear from examples 1 and 14 to 15, the brominated PC with the mass fraction of bromine within a specific range (20 to 22%) is selected, the initial impact strength of the obtained brominated flame-retardant PC/PBT alloy composition is higher (more than 701J/m), and the retention rate of the impact strength after aging by a xenon lamp is also higher (more than 81%).
As is clear from examples 1 and 16 to 18, the initial impact strength of the obtained brominated flame-retardant PC/PBT alloy composition is higher (697J/m or more) and the retention rate of impact strength after aging by a xenon lamp is also higher (82% or more) by selecting PBT with a proper viscosity (0.85 to 1.0 dl/g).
From examples 1, 19 and 20, it is known that the initial impact strength of the obtained brominated flame retardant PC/PBT alloy composition is higher and the retention rate of impact strength after aging by a xenon lamp is also higher by selecting the specific toughening agent (example 1) or the specific transesterification inhibitor (example 1).
The brominated PC6# is added in the comparative example 1, the initial decomposition temperature is too low, the retention rate of the impact strength of the obtained brominated flame-retardant PC/PBT alloy composition after aging of a xenon lamp is only 23%, and the impact strength is obviously reduced. In comparative example 2, brominated PC7# is added, only tetrabromobisphenol A is added in the preparation process of brominated PC7#, bisphenol A is not added, and the impact strength of the obtained brominated flame-retardant PC/PBT alloy composition is still obviously reduced after the xenon lamp is aged. In comparative example 3, brominated PC is not added, the initial flame retardant performance of the obtained brominated flame retardant PC/PBT alloy composition is poor, and the impact strength after ageing of a xenon lamp is obviously reduced; the brominated polycarbonate, brominated epoxy and brominated polystyrene are respectively added in comparative examples 4-6, the impact strength of the obtained brominated flame-retardant PC/PBT alloy composition is obviously reduced after the xenon lamp is aged, and the flame retardant property of the xenon lamps in comparative examples 5 and 6 is also deteriorated; the ratio of the sum of the mass of PC and brominated PC of comparative example 7 and comparative example 8 to the mass of PBT is not properly controlled, and the decrease in impact strength after xenon lamp aging of the obtained brominated flame retardant PC/PBT alloy composition is obvious.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (10)
1. The photoaging-resistant brominated flame-retardant PC/PBT alloy composition is characterized by comprising the following components in parts by weight:
the brominated PC is phosgene, tetrabromobisphenol A and a copolymer of bisphenol A; the initial decomposition temperature of the brominated PC is more than or equal to 460 ℃; the ratio of the sum of the masses of PC and brominated PC to the mass of PBT is 1: (0.2-0.7).
2. The brominated flame retardant PC/PBT alloy composition of claim 1, wherein the brominated PC has an initial decomposition temperature of 466 to 489 ℃.
3. The brominated flame-retardant PC/PBT alloy composition according to claim 1, wherein the mass fraction of bromine in the brominated PC is 20-22%.
4. The brominated flame retardant PC/PBT alloy composition of claim 1, wherein the PC has an average molecular weight of 25000 to 36000.
5. The brominated flame retardant PC/PBT alloy composition of claim 1, wherein the PBT has a viscosity of 0.85 to 1.0dl/g.
6. The brominated flame retardant PC/PBT alloy composition of claim 1, wherein the toughening agent is an acrylic-silicone rubber type toughening agent.
7. The brominated flame retardant PC/PBT alloy composition of claim 1, wherein the transesterification inhibitor is sodium dihydrogen phosphate.
8. The brominated flame retardant PC/PBT alloy composition of claim 1, further comprising 0.01 to 2 parts of a processing aid.
9. The method for preparing the brominated flame retardant PC/PBT alloy composition according to any one of claims 1 to 8, which is characterized by comprising the following steps: and mixing the components, melting, extruding and granulating to obtain the brominated flame-retardant PC/PBT alloy composition.
10. Use of the brominated flame retardant PC/PBT alloy composition of any of claims 1 to 8 in the preparation of low speed travel equipment products.
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