CN110628197A - Thin-wall flame-retardant polycarbonate/polyethylene glycol terephthalate alloy and preparation method thereof - Google Patents
Thin-wall flame-retardant polycarbonate/polyethylene glycol terephthalate alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a thin-wall flame-retardant polycarbonate/polyethylene glycol terephthalate alloy which comprises the following components in parts by weight: 50-80 parts of polycarbonate; 10-50 parts of polyethylene glycol terephthalate; 0.1-15 parts of a flame retardant; the polycarbonate has a weight average molecular weight of greater than 24000, a molecular weight distribution index (PDI) of less than 2.7, and a melt index stability evaluation MI% < 10%. According to the invention, by controlling the weight average molecular weight of the polycarbonate to be larger than, the molecular weight distribution index PDI and the melt index stability MI% to be larger than those of the common polycarbonate, the polycarbonate with the parameters has better compatibility with the polyethylene terephthalate, and the prepared alloy has better thin wall and flame retardant effect.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a thin-wall flame-retardant polycarbonate/polyethylene glycol terephthalate alloy and a preparation method thereof.
Background
Polycarbonate (PC) is a colorless and transparent amorphous thermoplastic material, and is widely used in many fields such as packaging, daily necessities, electronic and electric appliances, toys, instruments, transportation, and machine manufacturing because it is easily processed and suitable for various molding methods such as injection, extrusion molding, blow molding, etc., and has good mechanical and optical properties. Polyethylene terephthalate (PET) is a crystalline polyester and has the advantages of high heat resistance, high toughness, high fatigue resistance, self-lubrication, low friction coefficient and the like. However, PC also has a disadvantage of poor chemical resistance, and is difficult to be applied to equipment such as kitchen appliances and vehicles which are likely to be exposed to oil smoke. With the improvement of living standard, people have more and more strict requirements on the PC material with chemical resistance and flame retardant property.
The PC and the PET are blended to generate an alloy, so that the advantages of the PC and the PET can be combined, and the chemical resistance can be improved. However, after the PC and the PET are prepared into an alloy, the PET is often in an island shape and distributed in the PC as a discontinuous phase, which causes the filler and the additive to be selectively dissolved in the PC or the liquid crystal polyester due to different solubilities, resulting in insufficient performance (for example, poor thin-wall extrusion effect and reduced flame retardant effect).
As the market demand for flame retardant PC/PET alloys has grown year by year, most enterprises optimize the flame retardant properties of the alloys. However, the modification of flame retardant PC/PET alloys (or other flame retardant thermoplastic resins) by various enterprises is mainly focused on the formulation level, for example, chinese patent application 2019100237005 discloses a polycarbonate/crystalline polyester alloy in which a metal phosphate and a maleic anhydride polymer are added, so that the crystalline polyester can be continuously and uniformly distributed in PC, and the stability is improved.
Although the alloy with excellent performance can be obtained by optimizing the formula, if too much flame retardant is added to achieve the flame retardant effect and too much compatilizer is added to improve the compatibility of the two resins, the thin-wall flame retardant effect is often achieved, meanwhile, other performances are possibly reduced by adding too many types and too much flame retardant and compatilizer, and in order to meet other requirements, a plurality of other components are added, so that the cost is increased.
In summary, considering the microstructure of polycarbonate, it is important to consider the compatibility of polycarbonate with PET in a specific microstructure.
Disclosure of Invention
The invention aims to provide a thin-wall flame-retardant polycarbonate/polyethylene terephthalate alloy which has better thin-wall and flame-retardant performances by controlling the weight average molecular weight, the molecular weight distribution index PDI and the melt index stability of polycarbonate to evaluate MI%.
The invention also aims to provide a preparation method of the thin-wall flame-retardant polycarbonate/polyethylene terephthalate alloy.
The invention is realized by the following technical scheme
A thin-wall flame-retardant polycarbonate/polyethylene terephthalate alloy comprises the following components in parts by weight:
50-80 parts of polycarbonate;
10-50 parts of polyethylene terephthalate;
0.1-15 parts of a flame retardant;
the polycarbonate has a weight average molecular weight of greater than 18000, a molecular weight distribution index PDI of less than 2.7, and a melt index stability evaluation MI% < 10%.
Preferably, the polycarbonate has a weight average molecular weight 22000-26000, a molecular weight distribution index PDI of less than 2.2 and a melt index stability evaluation MI% < 8%.
Polycarbonate resins which meet the above-mentioned parametric characteristics may be branched thermoplastic polymers or copolymers obtained by reaction of dihydroxy compounds or mixtures thereof with small amounts of polyhydroxy compounds with phosgene (phosgene) or carbonic acid diesters. The production method of the polycarbonate resin is not particularly limited, and polycarbonate resins produced by a phosgene method (interfacial polymerization method) or a melting method (transesterification method) known so far may be used. An aromatic dihydroxy compound is preferable as the starting dihydroxy compound, and may be exemplified by 2, 2-bis (4-hydroxyphenyl) propane (═ bisphenol a), tetramethylbisphenol a, bis (4-hydroxyphenyl) -p-diisopropylbenzene, hydroquinone, resorcinol, 4-dihydroxybiphenyl and the like, of which bisphenol a is preferable. A compound in which at least one tetraalkylphosphonium sulfonate (tetraalkylphosphonium sulfonate) is bound to the aforementioned aromatic dihydroxy compound can also be used. Of the foregoing, the polycarbonate resin is preferably an aromatic polycarbonate resin derived from 2, 2-bis (4-hydroxyphenyl) propane, or an aromatic polycarbonate copolymer derived from 2, 2-bis (4-hydroxyphenyl) propane and other aromatic dihydroxy compounds. The polycarbonate resin may also be a copolymer in which the main component is an aromatic polycarbonate resin, for example, a copolymer with a polymer or oligomer containing a siloxane structure. Further, a mixture of two or more of the above polycarbonate resins may be used. The monohydric aromatic hydroxy compounds may be used to adjust the molecular weight of the polycarbonate resin, for example, m-methylphenol, p-methylphenol, m-propylphenol, p-t-butylphenol, and p- (long chain alkyl) -substituted phenols.
The method for producing the polycarbonate resin is not particularly limited in the present invention, and a polycarbonate resin produced by a phosgene method (interfacial polymerization method) or a melt method (transesterification method) can be used. The polycarbonate resin is also provided by subjecting the polycarbonate resin produced by the melt process to a post-treatment for adjusting the amount of terminal hydroxyl groups.
The molecular weight and molecular weight distribution index of the polycarbonate are mainly controlled by controlling the process conditions (such as feeding ratio, secondary feeding or multiple feeding, polymerization temperature and polymerization time). Melt index stability MI% is an index for evaluating the processing stability of polycarbonate, and mainly reflects whether there is an excessive amount of residual polymerization impurities in the polycarbonate, such as the molecular weight distribution of active reaction sites, etc., and impurities are removed during the post-treatment process after the polymerization is completed.
Polyethylene terephthalate is a polyester of terephthalic acid and ethylene glycol and is obtainable by polycondensation of dimethyl terephthalate and ethylene glycol, and also polycondensation of terephthalic acid and ethylene glycol. The ethylene glycol can be of biological origin, and the biological origin is mainly crop straws such as corn, sugarcane, wheat and the like. The polyethylene terephthalate may be modified and synthesized, and the diacid unit may further contain aromatic carboxylic acid ester derivatives such as dimethyl isophthalate, dimethyl isophthalate-5-sulfonate, dimethyl phthalate, dimethyl methyl terephthalate, dimethyl naphthalenedicarboxylate and dimethyl biphenyldicarboxylate, aliphatic polyesters such as dimethyl adipate, dimethyl pimelate, dimethyl suberate, dimethyl azelate and dimethyl dodecanedicarboxylate, and alicyclic dicarboxylic acid esters such as dimethyl cyclohexanedicarboxylate, dimethyl hexahydroisophthalate and dimethyl hexahydrophthalate.
The crystallinity of the polyethylene terephthalate is less than 15 percent;
preferably, the crystallinity of the polyethylene terephthalate is less than 10%. The crystallinity range of the common PET is 30-40%, and the PET with lower crystallinity is specially selected in the invention, so that the PET has better compatibility with PC, and the alloy has good thin wall and flame retardant property.
PET molecular weight is generally expressed in terms of viscosity.
The general molecular weight distribution of PET is determined by viscosity measurement, after drying treatment of PET resin, cleaning with acetone to remove surface water, placing in an oven at 100 ℃ for 10-15min to remove residual acetone, dissolving a sample in 110 ℃ oil bath, measuring the inner diameter of a viscometer capillary tube at 0.8-0.9mm, measuring the solution concentration at 0.005g/ml, and measuring by an automatic viscometer by adopting a mass ratio of phenol/tetrachloroethane of 1:1 as a solvent.
The testing method of the polycarbonate molecular weight distribution index PDI is gel permeation chromatography; the gel permeation chromatography analysis method specifically comprises the steps of respectively selecting 2mg of standard sample and a sample to be detected to be dissolved in 2ml of dichloromethane, filtering the solution by using a filter of a microporous filter membrane with the aperture of 0.45um after the solution is dissolved, setting the elution flow rate to be 1.0ml/min, setting the column temperature and the detection temperature to be 30 ℃, successively injecting standard sample solution and sample solution to be detected by using a sample injection syringe after a base line is stable, wherein the sample injection amount is 100ul, and performing elution through a chromatograph to obtain a final PDI result after the sample to be detected and the standard sample compare data.
The testing method for evaluating MI% of the polycarbonate melt index stability comprises the steps of weighing a certain amount of columnar particles, placing the columnar particles into a charging barrel of a melt index tester set to be 300 ℃, wherein the inner diameter of the charging barrel is 9.550mm, preheating 240s and 900s respectively, loading a 1.2kg weight, testing after a piston is pressed to a scale, cutting once every 10s to obtain 6 strips in total, recording the mass of the cut strips, and calculating to obtain MI a (melt index testing value under 240s testing condition) and MI b (melt index testing value under 900s testing condition), wherein MI% = (MI b-MI a)/a%.
The flame retardant is selected from at least one of a brominated flame retardant, a C1-C16 alkyl sulfonate flame retardant, a carbonate flame retardant, a fluorine-silver ion compound, a phosphorus flame retardant, a metal hydroxide flame retardant, an antimony-containing compound flame retardant synergist and a borate flame retardant.
The brominated flame retardant is selected from at least one of tetrabromobisphenol A, brominated triazine, brominated epoxy, decabromodiphenylethane, decabromodiphenyl ether, brominated polyimide, brominated polystyrene, polybrominated styrene, brominated polycarbonate and brominated polyacrylate;
the C1-C16 alkyl sulfonate flame retardant is selected from at least one of potassium perfluorobutyl sulfonate, potassium perfluorooctane sulfonate, tetraethylammonium perfluoroethane sulfonate and potassium diphenylsulfone sulfonate;
the carbonate flame retardant is selected from at least one of sodium carbonate, potassium carbonate, magnesium carbonate, calcium carbonate and barium carbonate;
the phosphorus flame retardant is at least one selected from phosphine flame retardants, hypophosphite flame retardants, phosphonite flame retardants, phosphite flame retardants, phosphine oxide flame retardants, hypophosphite flame retardants, phosphonate flame retardants, phosphate flame retardants, and polyphosphate flame retardants;
wherein the phosphine flame retardant may be phenoxyphosphazene; the phosphate ester flame retardant may be bisphenol a bis (diphenyl phosphate).
The metal hydroxide flame retardant is selected from at least one of magnesium hydroxide and aluminum hydroxide;
the borate flame retardant is at least one of anhydrous zinc borate, 3.5 hydrated zinc borate, alkali metal salts of boric acid and alkaline earth metal salts of boric acid.
0.1-5 parts of assistant is also included according to the parts by weight; the auxiliary agent is at least one of lubricant and antioxidant.
The lubricant is at least one selected from stearate lubricant, fatty acid lubricant and stearate lubricant; the stearate lubricant is at least one selected from calcium stearate, magnesium stearate and zinc stearate; the fatty acid lubricant is at least one selected from fatty acid, fatty acid derivative and fatty acid ester; the stearate lubricant is at least one selected from glyceryl monostearate and pentaerythritol stearate.
The antioxidant is organic phosphite ester, alkylated monophenol or polyhydric phenol, alkylation reaction product of polyhydric phenol and diene, butylated reaction product of p-cresol or dicyclopentadiene, alkylated hydroquinones, hydroxylated thiodiphenyl ethers, alkylene-bisphenol, benzyl compounds or polyhydric alcohol esters antioxidant.
Phosphite antioxidants such as antioxidant 168, antioxidant PEPQ, antioxidant PEP-36, antioxidant 9228, and the like.
The preparation method of the thin-wall flame-retardant polycarbonate/polyethylene terephthalate alloy comprises the following steps: adding the polycarbonate, the polyethylene glycol terephthalate, the flame retardant and the auxiliary agent into a high-speed mixer according to the proportion, uniformly mixing, adding into a double-screw extruder, extruding and granulating at the temperature of 220 ℃ and 250 ℃ to obtain the thin-wall flame-retardant polycarbonate/polyethylene glycol terephthalate alloy.
The invention has the following beneficial effects
The invention discovers that when the weight average molecular weight of the polycarbonate is more than 18000, the molecular weight distribution index PDI is less than 2.7, and the melt index stability evaluation MI% is less than 10%, the polycarbonate and PET have better compatibility compared with other polycarbonates, so that the prepared polycarbonate/polyethylene terephthalate alloy has better thin wall and flame retardant property.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
The sources of the raw materials used in the present invention are as follows, but are not limited by the following raw materials.
The following synthetic monomer for polycarbonate is bisphenol a.
Polycarbonate A: a weight average molecular weight of about 25000, a molecular weight distribution index PDI of 1.8, and a melt index stability evaluation MI% of 6.5%, prepared by a phosgene method, obtaining the set weight average molecular weight, PDI by controlling reaction parameters, and controlling the melt index stability evaluation MI by removing impurities during a post-treatment process at the end of polymerization;
polycarbonate B: a weight average molecular weight of about 20000, a molecular weight distribution index PDI of 2.3, and a melt index stability evaluation MI% of 8.3%, prepared by a phosgene method, obtaining the set weight average molecular weight and PDI by controlling reaction parameters, and controlling the melt index stability evaluation MI% by removing impurities during a post-treatment process after the polymerization is completed;
polycarbonate C: a weight average molecular weight of about 24000, a molecular weight distribution index PDI of 2.9, and a melt index stability evaluation MI% of 9.2%, prepared by a phosgene method, obtaining the set weight average molecular weight and PDI by controlling reaction parameters, and controlling the melt index stability evaluation MI by removing impurities during a post-treatment process at the end of polymerization;
polycarbonate D: a weight average molecular weight of about 17000, a molecular weight distribution index PDI of 2.3, and a melt index stability evaluation MI% of 8.4%, prepared by a phosgene method, obtaining the set weight average molecular weight and PDI by controlling reaction parameters, and controlling the melt index stability evaluation MI by removing impurities during a post-treatment process at the end of polymerization;
polycarbonate E: the weight average molecular weight is about 25000, the molecular weight distribution index PDI is 2.8, the melt index stability evaluation MI% is 14.3%, the preparation is carried out by a phosgene method, the set weight average molecular weight and PDI are obtained by controlling reaction parameters, and impurities are not removed by post-treatment;
PET-A: the crystallinity was 7.8%; the viscosity is 0.72;
PET-B: the crystallinity was 14%; the viscosity is 0.74;
PET-C: the crystallinity was 34%. The viscosity is 0.73;
flame retardant A: a phenoxyphosphazene;
and (3) a flame retardant B: bisphenol a bis (diphenyl phosphate);
lubricant: stearate based lubricants (PETS);
antioxidant: antioxidant 168, phosphite antioxidant;
a preparation method of polycarbonate/polyethylene terephthalate alloy comprises the following steps: adding the polycarbonate, the polyethylene glycol terephthalate, the flame retardant and the auxiliary agent into a high-speed mixer according to the proportion, uniformly mixing, and then adding into a double-screw extruder for extrusion and granulation at the temperature of 220 ℃ and 250 ℃ to obtain the polycarbonate/polyethylene glycol terephthalate alloy.
The performance test method comprises the following steps:
(1) flame retardant property: the polycarbonate composition was prepared as a 0.4mm film and tested for flame retardancy rating, test standard UL 94.
(2) Extrusion performance: forming a film with the thickness of 0.4mm by a fixed extrusion process, wherein the extrusion performance is better when the ratio of the tensile strength in the flow direction to the tensile strength perpendicular to the flow direction is the processing transverse-longitudinal tensile ratio and is closer to 1;
(3) appearance grade: 60 degree gloss test, characterizing the molded appearance rating.
Table 1: EXAMPLES composition ratios of polycarbonate/polyethylene terephthalate alloy and results of various property tests
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Polycarbonate A | 60 | 60 | 60 | |
| Polycarbonate B | 60 | |||
| PET-A | 40 | 40 | ||
| PET-B | 40 | 40 | ||
| Flame retardant A | 10 | 10 | 10 | |
| Flame retardant B | 10 | |||
| Lubricant agent | 0.2 | 0.2 | 0.2 | 0.2 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 |
| Flame retardant rating | V-0 | V-0 | V-0 | V-0 |
| Extrusion Properties | 0.98 | 0.78 | 0.77 | 0.93 |
| Appearance rating | 92 | 89 | 83 | 91 |
Table 2: comparative example polycarbonate/polyethylene terephthalate alloy composition ratios and Performance test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Polycarbonate A | 60 | |||
| Polycarbonate C | 60 | |||
| Polycarbonate D | 60 | |||
| Polycarbonate E | 60 | |||
| PET-A | 40 | 40 | 40 | |
| PET-C | 40 | |||
| Flame retardant A | 10 | 10 | 10 | 10 |
| Lubricant agent | 0.2 | 0.2 | 0.2 | 0.2 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 |
| Flame retardant rating | V-2 | V-2 | HB | V-2 |
| Extrusion Properties | 0.56 | 0.53 | 0.48 | 0.50 |
| Appearance rating | 78 | 71 | 56 | 53 |
As can be seen from examples 1-2 and comparative example 1, the crystallinity of PET greatly affects the compatibility of the flame retardant polycarbonate/PET alloy, which in turn affects the flame retardant properties, extrusion properties and appearance properties.
As can be seen from example 1/3 and comparative examples 2-4, the evaluation of the weight average molecular weight, molecular weight distribution index PDI, and melt index stability of the polycarbonate also greatly affected the performance of the flame retardant polycarbonate/PET alloy, with the flame retardant performance, extrusion performance, and appearance performance being the best within the preferred ranges.
Claims (9)
1. The thin-wall flame-retardant polycarbonate/polyethylene terephthalate alloy is characterized by comprising the following components in parts by weight:
50-80 parts of polycarbonate;
10-50 parts of polyethylene terephthalate;
0.1-15 parts of a flame retardant;
the polycarbonate has a weight average molecular weight of greater than 18000, a molecular weight distribution index PDI of less than 2.7, and a melt index stability evaluation MI% < 10%.
2. The thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy of claim 1, wherein the polycarbonate has a weight average molecular weight in the range of 22000-26000, a molecular weight distribution index PDI of less than 2.2, and a melt index stability assessment MI% < 8%.
3. The thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy according to claim 1 or 2, wherein the polycarbonate molecular weight distribution index PDI is measured by gel permeation chromatography; the gel permeation chromatography analysis method specifically comprises the steps of respectively selecting 2mg of standard sample and a sample to be detected to be dissolved in 2ml of dichloromethane, filtering the solution by using a filter of a microporous filter membrane with the aperture of 0.45um after the solution is dissolved, setting the elution flow rate to be 1.0ml/min, setting the column temperature and the detection temperature to be 30 ℃, injecting sample solution of the standard sample and the sample solution to be detected in sequence by using a sample injection syringe after a base line is stable, wherein the sample injection amount is 100ul, and performing elution on a chromatographic column to obtain the final PDI result after the sample to be detected and the standard sample compare data.
4. The thin-walled flame-retardant polycarbonate/polyethylene terephthalate alloy according to claim 1 or 2, wherein the method for testing the MI% of the polycarbonate melt index stability comprises weighing a certain amount of columnar particles, placing the columnar particles into a cylinder of a melt index tester set at 300 ℃, wherein the inner diameter of the cylinder is 9.550mm, preheating 240s and 900s respectively, loading a 1.2kg weight, pressing a piston to a scale, testing, cutting once every 10s, cutting 6 strips altogether, recording the mass of the cut strips, and calculating to obtain MI a (melt index test value under 240s test condition) and MI b (melt index test value under 900s test condition), and MI% = (MI b-MI a)/MI a%.
5. The thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy of claim 1 or 2, wherein the polyethylene terephthalate has a crystallinity of less than 15%; preferably, the crystallinity of the polyethylene terephthalate is less than 10%.
6. The thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy of claim 1 or 2, wherein the flame retardant is at least one selected from the group consisting of brominated flame retardants, C1-C16 alkyl sulfonate flame retardants, carbonate flame retardants, fluorine-silver ion complexes, phosphorus flame retardants, metal hydroxide flame retardants, antimony-containing compound flame retardant synergists, and borate flame retardants.
7. The thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy of claim 6, wherein the brominated flame retardant is selected from at least one of tetrabromobisphenol A, brominated triazine, brominated epoxy, decabromodiphenylethane, decabromodiphenyl ether, brominated polyimide, brominated polystyrene, polybrominated styrene, brominated polycarbonate, and brominated polyacrylate; the C1-C16 alkyl sulfonate flame retardant is selected from at least one of potassium perfluorobutyl sulfonate, potassium perfluorooctane sulfonate, tetraethylammonium perfluoroethane sulfonate and potassium diphenylsulfone sulfonate; the carbonate flame retardant is selected from at least one of sodium carbonate, potassium carbonate, magnesium carbonate, calcium carbonate and barium carbonate; the phosphorus flame retardant is at least one selected from phosphine flame retardants, hypophosphite flame retardants, phosphonite flame retardants, phosphite flame retardants, phosphine oxide flame retardants, hypophosphite flame retardants, phosphonate flame retardants, phosphate flame retardants, and polyphosphate flame retardants; the metal hydroxide flame retardant is selected from at least one of magnesium hydroxide and aluminum hydroxide; the borate flame retardant is at least one of anhydrous zinc borate, 3.5 hydrated zinc borate, alkali metal salts of boric acid and alkaline earth metal salts of boric acid.
8. The thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy of claim 1, further comprising 0.1 to 5 parts by weight of an auxiliary; the auxiliary agent is at least one of lubricant and antioxidant.
9. The method of making a thin-walled flame retardant polycarbonate/polyethylene terephthalate alloy of claim 8, comprising the steps of: adding the polycarbonate, the polyethylene glycol terephthalate, the flame retardant and the auxiliary agent into a high-speed mixer according to the proportion, uniformly mixing, adding into a double-screw extruder, extruding and granulating at the temperature of 220 ℃ and 250 ℃ to obtain the thin-wall flame-retardant polycarbonate/polyethylene glycol terephthalate alloy.
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| WO2021052088A1 (en) * | 2019-09-18 | 2021-03-25 | 金发科技股份有限公司 | Wall-thinning flame-retardant polycarbonate/polyethylene terephthalate alloy and preparation method therefor |
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| Publication number | Publication date |
|---|---|
| WO2021052088A1 (en) | 2021-03-25 |
| CN110628197B (en) | 2022-07-19 |
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