CN110746756B - Flame-retardant polycarbonate composite material and preparation method thereof - Google Patents
Flame-retardant polycarbonate composite material and preparation method thereof Download PDFInfo
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- 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
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- C08K5/5399—Phosphorus bound to nitrogen
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
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- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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Abstract
The invention discloses a flame-retardant polycarbonate composite material which comprises the following components in parts by weight: 60-100 parts of polycarbonate; 1-25 parts of a flame retardant; the weight average molecular weight of the polycarbonate is more than 26000, the molecular weight distribution index PDI is less than 2.2, the pH of the polycarbonate solution is 6.7-7.1, and the temperature change of Tg is realized through multiple cycles. It has been found in the present invention that when the polycarbonate is within the above parameters, the flame retardant has less effect on the stability of the polycarbonate.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a flame-retardant polycarbonate composite material and a preparation method thereof.
Background
Currently, Polycarbonate (PC) is widely used for producing various industrial and civil articles (such as various transparent articles, lamp covers, instrument panels, etc.). In order to expand the range of applications of polycarbonates, flame retardant modifications are required. However, since the polycarbonate is in a weak acid stable state, the addition of the flame retardant can change the overall pH value to affect the stability of the polycarbonate, and particularly, the alkali metal element (such as antimony dioxide) contained in the flame retardant and free bromine in the bromine flame retardant can cause the weak acid polycarbonate to be decomposed in the melt processing process, so that the performance of the polycarbonate is reduced, and even the performance of the polycarbonate cannot meet the application standard.
Generally, the method for improving the thermal stability of the flame retardant polycarbonate is to add a substance, for example, Chinese patent application 2018107637061 discloses a polycarbonate composition, wherein siloxane is added to improve the thermal stability of the flame retardant polycarbonate composition. Or, in order to ensure the stability of the flame-retardant polycarbonate, only some neutral and mild flame retardants can be added, so that the addition amount is large and the other properties of the material are greatly influenced.
There has been no report of a method for improving the stability of polycarbonate after adding a flame retardant by controlling the synthesis of polycarbonate to obtain polycarbonate within a specific parameter range.
Disclosure of Invention
The invention aims to provide a flame-retardant polycarbonate composite material which has the advantage of good thermal stability.
The invention also aims to provide a preparation method of the flame-retardant polycarbonate composite material.
The invention is realized by the following technical scheme:
the flame-retardant polycarbonate composite material comprises the following components in parts by weight:
60-100 parts of polycarbonate;
1-25 parts of a flame retardant;
the weight average molecular weight of the polycarbonate is more than 26000, the molecular weight distribution index PDI is less than 2.2, the pH of the polycarbonate solution is 6.7-7.1, and the temperature change of the multi-cycle Tg is less than 3.3 ℃.
Preferably, the polycarbonate has a weight average molecular weight of greater than 26000, a molecular weight distribution index PDI of less than 2.0, a polycarbonate solution pH of 6.8 to 6.9, and a multiple cycle Tg temperature change of less than 2.1 ℃.
Generally, the weight average molecular weight of more than 26000 belongs to the range from medium molecular weight to high molecular weight, and products with the molecular weight distribution index PDI of less than 2.2 and the temperature change of multiple cycle Tg of less than 3.3 ℃ are harder to obtain in the range; in general, the pH of the polycarbonate solution without pH adjustment is in the range of 6.3 to 7.3. The invention obtains the polycarbonate with corresponding molecular weight range and molecular weight distribution by refined and programmed reaction parameter control; the pH of the polycarbonate is also adjusted to 6.7-7.1 by adding hydroxide or acidic substances and the temperature change of the multi-cycle Tg is controlled to be less than 3.3 ℃ according to the relation between different molecular weights, molecular weight distribution and pH.
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 parameters of the polycarbonate product prepared by the process may be adjusted to meet the above-mentioned ranges of parameters.
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).
The method for testing the pH value of the polycarbonate solution comprises the steps of dissolving polycarbonate in a dichloromethane solvent, filtering the solution, and carrying out acid-base titration on an organic phase to test the pH value; the method of 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 leaching flow rate to be 1.0ml/min, setting the column temperature and the detection temperature to be 30 ℃, successively adding the standard solution and the sample to be detected into a sample injection syringe after a baseline is stable, leaching the sample injection amount to be 100ul by using an isochromatography, and obtaining the final PDI result after the sample to be detected and the standard sample are compared with data.
Generally, the pH of the polycarbonate solution is in the range of 6.3 to 7.3; the pH value range influencing the solution is mainly hydroxide in the raw materials, wherein the type of the hydroxide and the content of the hydroxide are the most critical factors, and the pH value range influencing the solution can be controlled by selecting and adding the hydroxide and can also be obtained by post-treatment and neutralization by added acid. The acid may be an organic acid such as citric acid, sulfonic acid, etc., or an organic acid such as phosphoric acid, phosphorous acid, etc.
The molecular weight distribution index PDI of polycarbonate, the purity of monomers in the polymerization process, catalyst residues, polymerization time, polymerization temperature and purification essence mode and process all have decisive influence on the molecular weight and the molecular weight distribution thereof, and on the same molecular weight level, the distribution index PDI =1 indicates that the molecular weight is uniform, generally, the PDI of the polymer is more than 1, the larger the PDI is, the distribution is wide, the smaller the PDI is, the distribution is approximately 1, and the distribution is narrow.
Multiple cycles Tg temperature change, glass transition, is a reversible transition of an amorphous region in an amorphous polymer or semi-crystalline polymer from a hard, relatively brittle glassy state to a viscous state or rubbery state during temperature rise, the glass transition temperature being the temperature at which the glass transition occurs. The uniformity of the polycarbonate can thus be verified by the Tg temperature change over a number of cycles. The uniformity of the polycarbonate resin means that the mobility of the macromolecular segment tends to be consistent in the process of repeatedly heating for many times, and the Tg temperature change is small, which indicates that the polycarbonate resin has good uniformity.
Tg temperature change test: on a relaxation-resistant polyma DSC214 NETSZSCH instrument, according to the D3418-15 ASTM standard, a temperature raising program is carried out after the temperature is set to be 20 ℃ and is kept for 30min, the temperature raising rate is 10 ℃/min, the temperature is immediately lowered after being raised to 200 ℃, after 3 times of round trip, one-time differential processing is carried out according to a heat signal of a curve, the initial Tg temperature and the third Tg temperature are obtained, and the two temperature differences are recorded as the change of the Tg temperature. Wherein, the smaller the Tg temperature change is, the better the stability of the composition is; conversely, the greater the change in Tg temperature, the less stable.
The flame retardant is at least one selected from C1-C16 alkyl sulfonate flame retardant, carbonate flame retardant, phosphorus flame retardant, metal hydroxide flame retardant, borate flame retardant and fluorine-silver ion compound.
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 polyphosphate flame retardant may be melamine polyphosphate.
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.
The flame retardant is at least one selected from C1-C16 alkyl sulfonate flame retardants.
0.1-5 parts of assistant is also included according to the parts by weight; the auxiliary agent is at least one selected from a lubricant, an antioxidant and an ultraviolet absorbent.
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 pentaerythritol stearate; preferably, the lubricant is at least one selected from fatty acid lubricants and stearate lubricants.
The ultraviolet absorbent is at least one selected from benzo triazine ultraviolet absorbent, bibenzoic acid ultraviolet absorbent and HALS compound.
The antioxidant can be hindered phenol antioxidant, phosphite antioxidant.
Phosphite antioxidants such as antioxidant 168, antioxidant PEPQ, antioxidant PEP-36, antioxidant 9228, and the like.
The preparation method of the flame-retardant polycarbonate composite material comprises the following steps: weighing the polycarbonate, the flame retardant and the auxiliary agent according to the proportion, uniformly mixing, adding into a double-screw extruder, and extruding and granulating (the temperature range of the screw is 200-280 ℃) to obtain the flame-retardant polycarbonate composite material.
Compared with the prior art, the invention has the following beneficial effects
The invention discovers that the stability of the polycarbonate (good flame retardant stability) can be reduced by overcoming the addition of a flame retardant when the polycarbonate meets a specific range by adjusting the weight average molecular weight, the molecular weight distribution index PDI, the pH value of a polycarbonate solution and the temperature change of multiple cycle Tg. Compared with the method for obtaining the stable flame-retardant polycarbonate composite material by adding other substances, the method has the advantages of lower cost, smaller influence on the performance of the polycarbonate and more contribution to further other modifications.
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 monomers for polycarbonate are bisphenol A and derivatives thereof
Polycarbonate A: the weight average molecular weight is about 27500, the molecular weight distribution index PDI is 2.1, the pH of a polycarbonate solution is 7.0, the temperature change of multi-cycle Tg is 3.0 ℃, the polycarbonate is prepared by a phosgene method, the set weight average molecular weight and PDI are obtained by controlling reaction parameters, and the pH value is adjusted and controlled by acid-base to obtain the temperature change of multi-cycle Tg;
polycarbonate B: the weight average molecular weight is about 28000, the molecular weight distribution index PDI is 1.7, the pH of a polycarbonate solution is 6.9, the temperature change of multi-cycle Tg is 2.0 ℃, the polycarbonate is prepared by a phosgene method, the set weight average molecular weight and PDI are obtained by controlling reaction parameters, and the pH is adjusted by acid-base to obtain the temperature change of multi-cycle Tg;
polycarbonate C: the weight average molecular weight is about 25000, the molecular weight distribution index PDI is 1.5, the pH of a polycarbonate solution is 7.0, the temperature change of multi-cycle Tg is 3.1 ℃, the polycarbonate is prepared by a phosgene method, the set weight average molecular weight and PDI are obtained by controlling reaction parameters, and the pH is regulated and controlled by acid-base to obtain the temperature change of multi-cycle Tg;
polycarbonate D: the weight average molecular weight is about 27000, the molecular weight distribution index PDI is 2.5, the pH of a polycarbonate solution is 7.2, the temperature change of multi-cycle Tg is 3.2 ℃, the polycarbonate is prepared by a phosgene method, the set weight average molecular weight and PDI are obtained by controlling reaction parameters, and the pH is adjusted and controlled by acid-base to obtain the temperature change of multi-cycle Tg;
polycarbonate E: the weight average molecular weight is about 28000, the molecular weight distribution index PDI is 2.6, the pH of a polycarbonate solution is 7.2, the temperature change of multi-cycle Tg is 4.0 ℃, the polycarbonate is prepared by a phosgene method, the set weight average molecular weight and PDI are obtained by controlling reaction parameters, and the pH is adjusted by acid-base to obtain the temperature change of multi-cycle Tg;
flame retardant A: a phenoxyphosphazene;
and (3) a flame retardant B: bisphenol a bis (diphenyl phosphate);
lubricant: stearate lubricants, PETS;
antioxidant: antioxidant 168, phosphite antioxidant;
examples and comparative examples a method of preparing a flame retardant polycarbonate composite: weighing the polycarbonate, the flame retardant and the auxiliary agent according to the proportion, uniformly mixing, adding into a double-screw extruder, and extruding and granulating (the temperature range of the screw is 200-280 ℃) to obtain the flame-retardant polycarbonate composite material.
The performance test method comprises the following steps:
(1) flame retardant rating: according to UL-94 standard, 1.5 mm.
(2) Flame retardant stability: putting the composition into an aging oven with the temperature set to 85 ℃ and the humidity set to 85 percent for accelerated aging for 500 hours, and testing the flame retardant property according to the UL-94 standard and 1.5 mm; the better the flame retardant stability, indicating the better the stability of the alloy.
(3) Long-term performance stability: according to f1 standard of UL 746B.
Table 1: EXAMPLES Components and Performance test results of flame-retardant polycarbonate composites
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Polycarbonate A | 100 | 100 | 100 | |
| Polycarbonate B | 100 | |||
| Flame retardant A | 10 | 20 | 10 | |
| Flame retardant B | 10 | |||
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 |
| Antioxidant agent | 0.01 | 0.01 | 0.01 | 0.01 |
| Flame retardant rating, 1.5mm | V-0 | V-0 | V-0 | V-0 |
| Stability of flame retardance | A- | A- | A- | A |
| Stability of long term performance | f1 | f1 | f1 | f1 |
Table 2: component proportion and performance test results of comparative example flame-retardant polycarbonate composite material
| Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Polycarbonate C | 100 | ||
| Polycarbonate D | 100 | ||
| Polycarbonate E | 100 | ||
| Flame retardant A | 10 | 10 | 10 |
| Lubricant agent | 0.5 | 0.5 | 0.5 |
| Antioxidant agent | 0.01 | 0.01 | 0.01 |
| Flame retardant rating, 1.5mm | V-2 | V-2 | V-2 |
| Stability of flame retardance | NG | NG | NG |
| Stability of long term performance | NG | NG | NG |
NG means the test failed.
As can be seen from examples 1 and 4, the preferred polycarbonates B are more flame-resistant and stable.
It can be seen from comparative examples 1-3 that the stability is poor when a flame retardant is added, which is reflected in poor flame retardancy, flame retardant stability and long term performance stability, without selecting polycarbonate in the range of the present invention.
Claims (8)
1. The flame-retardant polycarbonate composite material is characterized by comprising the following components in parts by weight:
60-100 parts of polycarbonate;
1-25 parts of a flame retardant;
the weight average molecular weight of the polycarbonate is more than 26000, the molecular weight distribution index PDI is less than 2.0, the pH of the polycarbonate solution is 6.7-7.1, and the temperature change of the multi-cycle Tg is less than 2.1 ℃.
2. The flame retardant polycarbonate composite of claim 1, wherein the polycarbonate has a pH of 6.8 to 6.9.
3. The flame retardant polycarbonate composite of claim 1 or 2, wherein the polycarbonate solution is tested for pH by dissolving the polycarbonate in a methylene chloride solvent, filtering the solution, and performing acid-base titration of the organic phase to test the pH; the method of molecular weight distribution index PDI is gel permeation chromatography.
4. The flame retardant polycarbonate composite of claim 1 or 2, wherein the flame retardant is at least one selected from the group consisting of a C1-C16 alkyl sulfonate flame retardant, a carbonate-based flame retardant, a phosphorus-based flame retardant, a metal hydroxide flame retardant, a borate flame retardant, and a fluorine-silver ion complex.
5. The flame retardant polycarbonate composite of claim 4, wherein the C1-C16 alkyl sulfonate flame retardant is selected from at least one of potassium perfluorobutyl sulfonate, potassium perfluorooctane sulfonate, tetraethylammonium perfluoroethane 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.
6. The flame retardant polycarbonate composite of claim 4, wherein the flame retardant is at least one selected from the group consisting of C1-C16 alkyl sulfonate flame retardants.
7. The flame retardant polycarbonate composite of claim 1 or 2, further comprising 0.1 to 5 parts by weight of an auxiliary; the auxiliary agent is at least one selected from a lubricant, an antioxidant and an ultraviolet absorbent.
8. The method of preparing a flame retardant polycarbonate composite of claim 7, comprising the steps of: weighing the polycarbonate, the flame retardant and the auxiliary agent according to the proportion, uniformly mixing, adding into a double-screw extruder, and extruding and granulating, wherein the temperature range of the screw is 200-280 ℃, so as to obtain the flame-retardant polycarbonate composite material.
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| CN111875943A (en) * | 2020-08-07 | 2020-11-03 | 宁波耀众模塑科技有限公司 | Carbon-containing high polymer material mixture for flame retardant for polyurethane foaming product |
| CN113637309B (en) * | 2021-08-17 | 2022-08-19 | 金发科技股份有限公司 | Flame-retardant polycarbonate alloy composition with high thermal stability and preparation method and application thereof |
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| CN107793722A (en) * | 2016-11-22 | 2018-03-13 | 金发科技股份有限公司 | A kind of polycarbonate compositions and preparation method thereof |
| CN109825056A (en) * | 2019-01-21 | 2019-05-31 | 金发科技股份有限公司 | A kind of polycarbonate alloy and preparation method thereof |
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| CN110746756A (en) | 2020-02-04 |
| WO2021052089A1 (en) | 2021-03-25 |
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