CN106317804A - 一种高透明度无卤阻燃材料 - Google Patents
一种高透明度无卤阻燃材料 Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 26
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 title abstract 4
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 34
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 15
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- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 claims abstract description 11
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims abstract description 5
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- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
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- YOLFSLXHLNWPKG-UHFFFAOYSA-N [3-bis(2,6-dimethylphenoxy)phosphoryloxyphenyl] bis(2,6-dimethylphenyl) phosphate Chemical compound CC1=CC=CC(C)=C1OP(=O)(OC=1C(=CC=CC=1C)C)OC1=CC=CC(OP(=O)(OC=2C(=CC=CC=2C)C)OC=2C(=CC=CC=2C)C)=C1 YOLFSLXHLNWPKG-UHFFFAOYSA-N 0.000 abstract 1
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- QLZHNIAADXEJJP-UHFFFAOYSA-L dioxido-oxo-phenyl-$l^{5}-phosphane Chemical compound [O-]P([O-])(=O)C1=CC=CC=C1 QLZHNIAADXEJJP-UHFFFAOYSA-L 0.000 abstract 1
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
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- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
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- 150000007942 carboxylates Chemical class 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
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- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
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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
- C08K5/00—Use of organic ingredients
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/50—Phosphorus bound to carbon only
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
本发明公开了一种高透明度无卤阻燃材料，涉及高分子材料领域。该阻燃材料是由以下重量份的原料组成：PETG树脂80～95份，阻燃剂5～20份，成核剂0.1～1份，抗氧剂0.1～1份；所述阻燃剂为无卤有机磷系阻燃剂，优选是由三苯基氧化膦、磷酸三苯酯、双酚A‑双(二苯基磷酸酯)、间苯二酚双(二苯基磷酸酯)、间苯二酚双[二(2,6‑二甲基苯基)磷酸酯]、聚苯基膦酸二苯砜酯中的至少两种组合而成。本发明使用的多种无卤阻燃剂，不影响PETG的透光性，保持PETG树脂透光度92％以上；低烟无卤，阻燃效果优异，UL94测试达到V‑0(3mm)，氧指数LOI大于30。本发明可广泛用于对阻燃以及透明性要求较高的建材、汽车、电子以及纺丝等领域。
Description
技术领域
本发明涉及高分子材料领域，具体涉及一种高透明度无卤阻燃材料。
背景技术
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯(PETG)是一种透明、非结晶型共聚酯，它是由对苯二甲酸(PTA)、乙二醇(EG)和1,4-环己烷二甲醇(CHDM)三种单体用酯交换法缩聚的产物。PETG与PET比较多了1,4-环己烷二甲醇共聚单体，与PCT比较多了乙二醇共聚单体，因此，PETG的性能和PET、PCT大不相同。PETG板材具有突出的韧性和高抗冲击强度，其抗冲击强度是改性聚丙烯酸酯类的3～10倍，并具有很宽的加工范围，高的机械强度和优异的柔性，比起PVC透明度高，光泽好，容易印刷，是新一代的环保塑料。
由于PETG的氧指数只有25％左右，容易被引燃并且在空气中持续持燃烧，同时伴随有熔滴和流延起火现象，产生大量的不饱和气体，严重限制了其应用范围。随着PETG的应用领域越来越广，带来的火灾危险也就越大，因此对PETG材料进行阻燃改性是十分必要的。通过查阅资料很少有对PETG材料进行阻燃改性的报道。
发明内容
本发明的目的在于提供一种高透明度无卤阻燃材料，该阻燃材料具有高透明度、无卤环保、阻燃效果好等优点。
本发明所采用的技术解决方案是：
一种高透明度无卤阻燃材料，其是由以下重量份的原料组成：PETG树脂80～95份，阻燃剂5～20份，成核剂0.1～1份，抗氧剂0.1～1份；所述阻燃剂为无卤有机磷系阻燃剂。
优选的，所述无卤有机磷系阻燃剂是由烷基氧化膦以及有机磷酸酯中的至少两种组合而成。
上述无卤有机磷系燃剂优选采用下述结构：
其中：R1，R2，R3为独立地选自碳原子数为1-18的烷基、烷氧基、芳基、芳氧基；R4，R5，R6，R7，R8,A为独立地选自碳原子数为1-18的烷基或者芳基，n1为1-10，n2为1-100。
优选的，上述无卤有机磷系阻燃剂是由三苯基氧化膦、磷酸三苯酯、双酚A-双(二苯基磷酸酯)、间苯二酚双(二苯基磷酸酯)、间苯二酚双[二(2,6-二甲基苯基)磷酸酯]、聚苯基膦酸二苯砜酯中的至少两种组合而成。
更加优选的，所述无卤有机磷系阻燃剂是由三苯基氧化膦、双酚A-双(二苯基磷酸酯)和聚苯基膦酸二苯砜酯组成。
优选的，所述成核剂为羧酸盐类、山梨醇类以及高分子类成核剂中的一种或者两种的组合。
更加优选的，所述成核剂为苯甲酸钠。
优选的，所述抗氧剂由受阻酚类抗氧剂和有机亚磷酸酯抗氧剂组成。
更加优选的，所述抗氧剂由PEPQ抗氧剂和1010抗氧剂组成，PEPQ抗氧剂和1010抗氧剂的质量比为1:1。
本发明的有益技术效果是：
本发明采用烷基氧化膦以及磷酸酯类多种阻燃剂对PETG进行阻燃改性，同时加入适量的成核剂以及抗氧剂助剂，制得的阻燃材料低烟无卤，阻燃效果优异，垂直燃烧达到V-0(3mm)，氧指数大于30，并且透光率高，最大限度的保留了PETG的透明度。本发明提升了PETG的应用效果，拓宽了其应用领域(可广泛用于对阻燃以及透明性要求较高的建材、汽车、电子以及纺丝等领域)，具有很好的实用价值与推广前景。
具体实施方式
下面结合具体实施例来对本发明作进一步说明。
实施例1
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 83份，阻燃剂三苯基氧化膦TPO 15份，成核剂苯甲酸钠NaA 1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
将称量好的各原料干燥，然后加入高速混料机中混合10min，取出，加入到熔融温度为150-240℃的双螺杆挤出机中挤出，造粒，即可得到本发明高透明度无卤阻燃材料。双螺杆挤出机的工艺条件为：挤出机一区温度140-160℃，二区温度160-180℃，三区温度180-200℃，四区温度200-220℃，五区温度220-240℃，六区温度220-240℃，七区温度220-240℃，八区温度220-240℃，机头温度220-230℃，主机转速100rpm，喂料速度30rpm，物料在螺杆中的输送时间为1-2min。
实施例2
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 83份，阻燃剂磷酸三苯酯15份，成核剂苯甲酸钠NaA 1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
实施例3
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 88份，阻燃剂三苯基氧化膦TPO 5份，阻燃剂双酚A-双(二苯基磷酸酯)BDP 5份，成核剂苯甲酸钠1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
实施例4
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 88份，阻燃剂磷酸三苯酯TPP5份，阻燃剂间苯二酚双(二苯基磷酸酯)RDP 5份，成核剂苯甲酸钠NaA 1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
实施例5
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 88份，阻燃剂三苯基氧化膦TPO 5份，阻燃剂聚苯基膦酸二苯砜酯PSPPP 5份，成核剂苯甲酸钠NaA 1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
实施例6
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 90份，阻燃剂三苯基氧化膦TPO 2份，阻燃剂双酚A-双(二苯基磷酸酯)BDP 3份，阻燃剂聚苯基膦酸二苯砜酯PSPPP 3份，成核剂苯甲酸钠NaA 1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
实施例7
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 90份，阻燃剂三苯基氧化膦TPO 2份，阻燃剂双酚A-双(二苯基磷酸酯)BDP 3份，阻燃剂聚苯基膦酸二苯砜酯PSPPP 3份，成核剂滑石粉Talc 1份，PEPQ抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
实施例8
按下述重量份配比称取各原料：
聚对苯二甲酸乙二醇酯-1,4-环己烷二甲醇酯PETG 90份，阻燃剂三苯基氧化膦TPO 2份，阻燃剂双酚A-双(二苯基磷酸酯)BDP 3份，阻燃剂聚苯基膦酸二苯砜酯PSPPP 3份，成核剂苯甲酸钠NaA 1份，168抗氧剂0.5份，1010抗氧剂0.5份。
制备方法同实施例1。
性能评价方式及实行标准
将上述实施例1～8中完成造粒的粒子在60-70℃的鼓风干燥箱中干燥4～6小时，再将干燥后的粒子在100T注塑机上制样，制样过程中保持模温30～80℃之间。
塑料透光度按照GB/T2410-2008标准进行检验，试样尺寸(mm)(50)×(50)的方片；垂直燃烧测试按照GB/T2408-2008标准，试样尺寸(mm)(125±5)×(13.0±0.5)×(3±0.25)；氧指数按照GB/T2404.2-2009标准，试样类型IV，尺寸(mm)(80±5)×(6.5±0.5)×(3±0.25)。
上述实施例1～8中制得的阻燃材料的性能如下表1。
表1
由表1可看出，本发明制得的阻燃材料阻燃效果优异，透光率高。尤其是实施例6给出的配方体系，所制得的阻燃材料既可以垂直燃烧UL94达到V-0级，氧指数32％，并且可以保持透光率93％。
Claims (10)
1.一种高透明度无卤阻燃材料，其特征在于它是由以下重量份的原料组成：PETG树脂80～95份，阻燃剂5～20份，成核剂0.1～1份，抗氧剂0.1～1份；所述阻燃剂为无卤有机磷系阻燃剂。
2.根据权利要求1所述的一种高透明度无卤阻燃材料，其特征在于：所述无卤有机磷系阻燃剂是由烷基氧化膦以及有机磷酸酯中的至少两种组合而成。
3.根据权利要求1所述的一种高透明度无卤阻燃材料，其特征在于，所述无卤有机磷系阻燃剂采用下述结构：
其中：R1，R2，R3为独立地选自碳原子数为1-18的烷基、烷氧基、芳基或者芳氧基；R4，R5，R6，R7，R8，A为独立地选自碳原子数为1-18的烷基或者芳基，n1为1-10，n2为1-100。
4.根据权利要求1、2或3所述的一种高透明度无卤阻燃材料，其特征在于：所述无卤有机磷系阻燃剂是由三苯基氧化膦、磷酸三苯酯、双酚A-双(二苯基磷酸酯)、间苯二酚双(二苯基磷酸酯)、间苯二酚双[二(2,6-二甲基苯基)磷酸酯]、聚苯基膦酸二苯砜酯中的至少两种组合而成。
5.根据权利要求4所述的一种高透明度无卤阻燃材料，其特征在于：所述无卤有机磷系阻燃剂是由三苯基氧化膦、双酚A-双(二苯基磷酸酯)和聚苯基膦酸二苯砜酯组成。
6.根据权利要求1所述的一种高透明度无卤阻燃材料，其特征在于：所述成核剂为羧酸盐类、山梨醇类以及高分子类成核剂中的一种或者两种的组合。
7.根据权利要求6所述的一种高透明度无卤阻燃材料，其特征在于：所述成核剂为苯甲酸钠。
8.根据权利要求1所述的一种高透明度无卤阻燃材料，其特征在于：所述抗氧剂由受阻酚类抗氧剂和有机亚磷酸酯抗氧剂组成。
9.根据权利要求8所述的一种高透明度无卤阻燃材料，其特征在于：所述抗氧剂由PEPQ抗氧剂和1010抗氧剂组成。
10.根据权利要求9所述的一种高透明度无卤阻燃材料，其特征在于：所述PEPQ抗氧剂和1010抗氧剂的质量比为1:1。
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