WO2020151553A1 - Alliage de polycarbonate et procédé de préparation s'y rapportant - Google Patents

Alliage de polycarbonate et procédé de préparation s'y rapportant Download PDF

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Publication number
WO2020151553A1
WO2020151553A1 PCT/CN2020/072290 CN2020072290W WO2020151553A1 WO 2020151553 A1 WO2020151553 A1 WO 2020151553A1 CN 2020072290 W CN2020072290 W CN 2020072290W WO 2020151553 A1 WO2020151553 A1 WO 2020151553A1
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Prior art keywords
flame retardant
polycarbonate
polycarbonate alloy
hypophosphite
acid
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PCT/CN2020/072290
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English (en)
Chinese (zh)
Inventor
艾军伟
岑茵
黄险波
叶南飚
董相茂
王培涛
陈勇文
丁超
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金发科技股份有限公司
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Publication of WO2020151553A1 publication Critical patent/WO2020151553A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
    • C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates

Definitions

  • the invention relates to the technical field of polymer composite materials, in particular to a polycarbonate alloy and a preparation method thereof.
  • PC polycarbonate
  • PC and ABS are very sensitive to metals, especially heavy metals such as silver.
  • the presence of heavy metals can greatly accelerate the degradation of ABS and PC.
  • effective antibacterial agents mainly contain silver ions, and silver ions are subject to shear, heat, and environmental factors during processing and use.
  • the effective components of silver ion antibacterial agents are easily converted to more alkaline ones. Its oxide not only loses antibacterial properties and the alloy color turns gray, but also further deteriorates the alloy.
  • ABS/PC flame retardant alloys are prepared, and the addition of flame retardants will affect the stability of the alloy, and if the alloy system is in an unstable state, it will also affect the flame retardant performance.
  • flame retardants will affect the stability of the alloy, and if the alloy system is in an unstable state, it will also affect the flame retardant performance.
  • bromine-antimony flame retardant systems cannot be added to PC, because the free bromine and alkaline antimony compounds can degrade the stability of the alloy, and the high temperature during processing will aggravate the deterioration of the alloy. The processing window is shorter.
  • Chinese patent 201611189108.5 discloses a PC/ABS alloy with excellent thermal aging properties, in which 0.1-2 parts of phosphate ester is used to adjust the pH value of the alloy to 6.6-8.2, and epoxy resin is used to cap the PC.
  • the PC/ABS alloy obtained after auxiliary use meets the long-term thermal aging requirements of 100 degrees and 1000 hours.
  • the core of the invention is to use epoxy resin to cap the PC, so that the alloy can still obtain good thermal stability when the pH is alkaline, especially When the pH value of Example 3 is 8.2, good heat aging resistance can still be obtained.
  • the pH adjuster used is phosphoric acid ester (triphenyl phosphite, sodium dihydrogen phosphate, sodium dihydrogen phosphite).
  • Phosphate esters include triphenyl phosphate used as a flame retardant, etc., triphenyl phosphite Usually exists as a heat stabilizer. Sodium dihydrogen phosphate and sodium dihydrogen phosphite are mainly used to improve the stability of the ester group in the melt during processing. Therefore, it can be seen that the "phosphate ester" added by the patent cannot function alone in this system. On the other hand, using epoxy resin to cap the PC will increase the alkalinity of the alloy.
  • this patent mainly uses epoxy resin to cap the PC to increase the thermal stability of the system.
  • the pH regulator used in this patent is a weak Lewis acid, and the added amount is large, which easily affects other properties (such as impact strength and stress cracking properties).
  • Triphenyl phosphite, sodium dihydrogen phosphate, and sodium dihydrogen phosphite are in the form of solid powders or fine particles. Due to the small amount used, it is difficult to uniformly disperse in the alloy, causing difficulties in processing.
  • the purpose of the present invention is to provide a polycarbonate alloy which has the advantages of moist heat stability, a wider processing window and the like.
  • Another object of the present invention is to provide a method for preparing the above polycarbonate alloy.
  • a polycarbonate alloy in parts by weight, including the following components:
  • the pH value of the polycarbonate alloy is 6.3-6.9, and the pH value is adjusted by liquid acid.
  • the liquid acid is selected from at least one of phosphoric acid and acetic acid.
  • the main function of the liquid acid is to stably mix into the polycarbonate alloy in the melt state and stabilize the acid-base balance of the alloy melt during processing.
  • Phosphoric acid and acetic acid are more commonly used acid regulators.
  • the present invention uses liquid acid to adjust the pH value of the polycarbonate alloy. Because the acidity is stronger than that of Lewis acids, it only needs one part per thousand or less of the actual content to reach the target pH value. These acids will Evenly dispersed in the alloy, it will not affect other properties of the alloy.
  • the acidity of liquid acid is relatively strong, so the actual amount of liquid acid added during alloy pH adjustment is difficult to calculate based on the target pH value, and the high temperature in the screw can easily volatilize the liquid acid quickly, making the liquid acid entering the alloy Can not get expectations and control. Therefore, if the liquid acid is effectively incorporated into the alloy, it is a technical difficulty that plagues the present invention.
  • the present invention uses porous foamed polycarbonate or porous foamed ABS, which contains liquid acid, which can effectively make the liquid acid into the alloy in the screw, and the effective liquid acid will be evenly dispersed. In the alloy resin, excess liquid acid will volatilize.
  • the pH value points obtained by testing the addition amount of n liquid acid are drawn into a pH-liquid acid addition amount curve.
  • the more test points n the more accurate the curve, and the drawn curve obtains the addition amount of the liquid acid at the target pH value. After a few attempts to obtain the alloy product of the target pH.
  • the polycarbonate resin of the present invention may be a branched thermoplastic polymer or copolymer obtained by the reaction of a dihydroxy compound or a small amount of a polyhydroxy compound with phosgene or a carbonic acid diester.
  • the production method of the polycarbonate resin is not particularly limited, and the polycarbonate resin produced by the hitherto known phosgene method (interfacial polymerization method) or melting method (transesterification method) can be used.
  • bisphenol A 2,2-bis(4-hydroxyphenyl)propane
  • tetramethylbisphenol A bis(4-hydroxyphenyl) )-P-diisopropylbenzene
  • hydroquinone resorcinol
  • 4,4-dihydroxydiphenyl etc.
  • a compound in which at least one tetraalkylphosphonium sulfonate is bonded to the aforementioned aromatic dihydroxy compound can also be used.
  • the polycarbonate resin is preferably an aromatic polycarbonate resin derived from 2,2-bis(4-hydroxyphenyl)propane, or from 2,2-bis(4-hydroxyphenyl)propane and other aromatics.
  • the polycarbonate resin may also be a copolymer in which the main composition is an aromatic polycarbonate resin, for example, a copolymer with a siloxane structure-containing polymer or oligomer.
  • a mixture of two or more of the aforementioned polycarbonate resins may be used.
  • Monovalent aromatic hydroxy compounds can be used to adjust the molecular weight of polycarbonate resins, for example, m-cresol, p-cresol, m-propyl phenol, p-propyl phenol, p-tert-butyl phenol and p-(long chain alkyl )-Substituted phenol.
  • the present invention has no particular limitation on the production method of the polycarbonate resin, and the polycarbonate resin produced by the phosgene method (interfacial polymerization method) or the melting method (transesterification method) can be used.
  • the polycarbonate resin is also provided by subjecting a polycarbonate resin produced by a melt method to a post-treatment for adjusting the amount of terminal hydroxyl groups.
  • ABS acrylonitrile-butadiene-styrene copolymer refers to acrylonitrile which can be a blend of acrylonitrile-butadiene-styrene terpolymer or styrene-butadiene rubber and styrene-acrylonitrile copolymer -Butadiene-styrene polymer.
  • the present invention has no special requirements for the content of each section, and the content of acrylonitrile can be 11-36%, the content of butadiene is 8-36%, and the content of styrene is 28-80%.
  • the pH of the polycarbonate prepared according to different raw materials, different preparation processes, synthesis residues, and different end-capping groups is between 6.2 and 7.3.
  • polycarbonate is mixed with ABS, other additives, and fillers to prepare an alloy, it will further change the pH of the alloy. If the final pH of the alloy (especially mineral filling, antibacterial silver ion filling, and the addition of a large amount of flame retardant) is not in the weak acid range of 6.3-6.9, it will seriously affect the stability of the alloy, especially the shear during melt extrusion. Make the degradation of molecules serious.
  • the silver ion antibacterial agent alloy is prepared, based on the total weight of the polycarbonate alloy, and also includes silver ions with a content of 100-1200 ppm.
  • Silver ions are derived from silver ion antibacterial agents. At this time, it is not only necessary to consider the destabilization effect of the residual substances in ABS, but also the stability of silver ions. Within the range of 6.3-6.9, the stability of silver ions is strong and the remaining impurities in ABS are effectively suppressed, making the alloy It has good antibacterial performance and good humidity and heat stability. These stability are not only reflected in the range of daily use, but also in the stability of the processing process, thus providing a wider processing window.
  • flame-retardant polycarbonate alloy If it is necessary to prepare a flame-retardant polycarbonate alloy, it also includes 0-15 parts by weight of flame retardant.
  • the flame retardant is selected from bromine flame retardants, C1-C16 alkyl sulfonate flame retardants, carbonate flame retardants, fluorine-silver ion composites, phosphorus flame retardants, metal hydroxides 1. At least one of antimony-containing compound flame retardant synergist and borate flame retardant;
  • the brominated flame retardant is selected from tetrabromobisphenol A, brominated triazine, brominated epoxy, decabromodiphenyl ethane, decabromodiphenyl ether, brominated polyimide, brominated polyphenylene At least one of ethylene, polybrominated styrene, brominated polycarbonate, and brominated polyacrylate;
  • the C1-C16 alkyl sulfonate flame retardant is selected from potassium perfluorobutane sulfonate, potassium perfluorooctane sulfonate, tetraethyl ammonium perfluoroethane sulfonate, potassium diphenylsulfone sulfonate At least one of
  • the carbonic acid 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 selected from phosphine flame retardant, hypophosphite flame retardant, hypophosphite flame retardant, phosphonite flame retardant, phosphonite flame retardant, phosphite Flame retardant, phosphite flame retardant, phosphine oxide flame retardant, hypophosphite flame retardant, hypophosphite flame retardant, phosphonate flame retardant, phosphonate flame retardant, phosphate flame retardant , At least one of 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 selected from at least one of anhydrous zinc borate, 3.5 water zinc borate, alkali metal salts of boric acid, and alkaline earth metal salts of boric acid.
  • the hypophosphite flame retardant is selected from at least one of aluminum hypophosphite, calcium hypophosphite, dimethyl aluminum hypophosphite, diethyl aluminum hypophosphite, and methyl ethyl aluminum hypophosphite;
  • the flame retardant is selected from bisphenol A bis (diphenyl phosphate), phenoxy phosphazene, resorcinol (diphenyl phosphate), triphenyl phosphate, melamine polyphosphate, and melamine cyanurate
  • the polyphosphate flame retardant is selected from at least one of ammonium polyphosphate, melamine phosphate, melamine pyrophosphate, and melamine polyphosphate.
  • the flame retardant is selected from phosphorus flame retardants
  • the phosphorus flame retardant is selected from phosphate flame retardants
  • the phosphate ester flame retardant is selected from phenoxyphosphazene.
  • it also includes 0-5 parts of at least one of antioxidants, weathering agents, and pigments.
  • the lubricant is selected from at least one of stearate lubricants, fatty acid lubricants, and stearate lubricants;
  • the stearate lubricant is selected from at least one of calcium stearate, magnesium stearate, and zinc stearate;
  • the fatty acid lubricant is selected from fatty acids, fatty acid derivatives, and fatty acid esters At least one;
  • the stearate lubricant is selected from at least one of pentaerythritol stearate.
  • the above-mentioned preparation method of polycarbonate alloy includes the following steps: adding polycarbonate, ABS resin, porous foamed polycarbonate with liquid acid or porous foamed ABS to a high-speed mixer, and then add to In a twin-screw extruder, melt and mix at a temperature of 230-250°C, then pelletize, cool, and dry to obtain a polycarbonate alloy.
  • the present invention inhibits the cracking effect of residual impurities in the ABS resin, especially residual emulsifiers, ensures the stability of the alloy, and also improves the extrusion and melting process.
  • the stability of the machine broadens the processing window.
  • the silver ion antibacterial polycarbonate alloy system is prepared, and the pH adjustment by using liquid acid not only improves the stability of the alloy, but also improves the stability of the silver ion.
  • a stable alloy system can promote the stability of silver ions (reflected by a good antibacterial effect and good color stability), and the stability of silver ions also promotes the improvement of the stability of the alloy system. Therefore, the obtained silver ion antibacterial polycarbonate alloy has good antibacterial effect and stability, and also widens the processing window.
  • Figure 1 Schematic diagram of the zodiac grid evaluation method.
  • the sources of the raw materials used in the present invention are as follows, but are not limited by the following raw materials.
  • Silver ion source silver ion antibacterial agent, IKM50G, Japan Zeomic;
  • Liquid acid phosphoric acid
  • Flame retardant B bisphenol A bis (diphenyl phosphate);
  • Flame retardant C melamine polyphosphate
  • Lubricant stearate lubricant, PETS;
  • Example Preparation method of polycarbonate alloy Add polycarbonate, ABS resin, silver ion antibacterial agent, porous foamed polycarbonate with liquid acid or porous foamed ABS, and flame retardant to high-speed mixing according to the ratio.
  • the material is evenly mixed in the feeder, then added to the twin-screw extruder, melted and mixed at a temperature of 230-250°C, then pelletized, cooled and dried to obtain a polycarbonate alloy.
  • Alloy pH Dissolve the composition in a methylene chloride solvent, filter the solution, and perform acid-base titration of the organic phase to test the pH.
  • Processing window using the twelve grid evaluation method, under the condition of fixed injection pressure and back pressure, the injection temperature is divided into 250°C, 280°C, 300°C, 320°C, and the injection speed is divided into high and medium , Low speed, so the formation of different injection molding processing window areas, evaluate the appearance quality, mechanical performance stability, and processing screw rotation state of injection molded parts under different area windows. If the above properties can be combined, it means the processing The window is satisfied, and the more the number of regions is satisfied, the wider the processing window, the best is 12, and the worst is 0; the zodiac grid is shown in Figure 1.
  • ICP standard curve extrapolation method The Ag content in the composition is determined by optical emission spectroscopy with inductively coupled plasma (ICP-OES). In order to determine the total Ag content, weigh 2g. The composition was measured, treated with 5ml of nitric acid and stirred for trial production to dissolve, and the solution was supplemented to 100ml, and the total Ag content was calculated by the ICP standard curve extrapolation method.
  • ICP-OES inductively coupled plasma
  • Flame-retardant stability Put the composition into an aging box with a temperature of 85°C and a humidity of 85% for accelerated aging for 500 hours, and then test the flame-retardant performance according to the UL-94 standard at 1.5mm; flame-retardant stability The better, the better the stability of the alloy.
  • Example 1-4 and Comparative Example 1-2 each group distribution ratio (weight parts) and various performance test results
  • the pH value of the polycarbonate alloys of Examples 1-4 and Comparative Example 1-2 without adjusting the pH is 7.1
  • the pH value of the alloys of Examples 1-4 and Comparative Example 2 in Table 1 is obtained by adding Liquid acid regulator is adjusted.
  • Table 2 The distribution ratio (weight parts) of each group of Examples 5-8 and Comparative Examples 3-4 and the results of each performance test
  • Table 3 The distribution ratio (parts by weight) of each group of Examples 9-11 and Comparative Examples 5-6 and the results of each performance test
  • the pH of the polycarbonate alloys of the Examples and Comparative Examples under the premise of not adjusting the pH is 7.0, and the pH values of the alloys of the Examples and Comparative Examples in Table 3 are adjusted by adding a liquid acid regulator .

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne un alliage de polycarbonate, comprenant les constituants suivants, en parties en poids : 70 parties de polycarbonate et de 1 à 60 parties d'une résine ABS. La valeur de pH de l'alliage de polycarbonate est de 6,3 à 6,9 et peut être ajustée au moyen d'un acide liquide. Dans la présente invention, l'ajustement de la valeur de pH de l'alliage de polycarbonate permet à l'alliage de polycarbonate de la présente invention de présenter des avantages tels qu'une bonne stabilité à la chaleur humide et une grande fenêtre de traitement.
PCT/CN2020/072290 2019-01-21 2020-01-15 Alliage de polycarbonate et procédé de préparation s'y rapportant WO2020151553A1 (fr)

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CN113583423A (zh) * 2021-08-17 2021-11-02 广州仕天材料科技有限公司 一种高流动性阻燃pc/abs复合材料及其制备方法

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CN109825056B (zh) * 2019-01-21 2022-07-19 金发科技股份有限公司 一种聚碳酸酯合金及其制备方法
CN110643162B (zh) * 2019-09-18 2021-11-16 广东金发科技有限公司 一种聚碳酸酯/abs合金及其制备方法
CN110746756B (zh) * 2019-09-18 2021-08-20 金发科技股份有限公司 一种阻燃聚碳酸酯复合材料及其制备方法
CN111117184A (zh) * 2019-12-17 2020-05-08 中广核俊尔(浙江)新材料有限公司 一种耐高温高湿的阻燃pc塑料及其制备方法和应用
CN111320857A (zh) * 2020-04-20 2020-06-23 上海瑞昱实业有限公司 一种抗静电抗菌无卤阻燃pc/abs组合物及其制备方法
CN112662037B (zh) * 2020-11-30 2022-05-20 金发科技股份有限公司 一种高性能高阻燃聚乙烯滚塑专用料及其制备方法和应用

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