WO2023160154A1 - 一种pbt/pet复合材料及其制备方法和应用 - Google Patents

一种pbt/pet复合材料及其制备方法和应用 Download PDF

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WO2023160154A1
WO2023160154A1 PCT/CN2022/139529 CN2022139529W WO2023160154A1 WO 2023160154 A1 WO2023160154 A1 WO 2023160154A1 CN 2022139529 W CN2022139529 W CN 2022139529W WO 2023160154 A1 WO2023160154 A1 WO 2023160154A1
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pbt
composite material
pet composite
acetaldehyde
pet
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PCT/CN2022/139529
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French (fr)
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朱文
陈平绪
叶南飚
莫文杰
付学俊
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金发科技股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K5/00—Casings, cabinets or drawers for electric apparatus
    • H05K5/02—Details
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/06—Biodegradable
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/22—Halogen free composition

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  • the invention relates to the technical field of polymer materials, in particular to a PBT/PET composite material and its preparation method and application.
  • Polybutylene terephthalate PBT has excellent electrical properties, mechanical strength and processability due to its crystallization and linear saturation.
  • the modified polyester has been widely used in the fields of electronics and electricity.
  • Halogen-free flame-retardant glass fiber-reinforced PBT is often used as components such as cooling fan frame blades, motor casings, relays, connectors, etc., and has gained a lot of recognition in the industry;
  • polyethylene terephthalate PET has With high melting point (Tm) and glass transition temperature (Tg), it is also a linear saturated crystalline polymer, and maintains excellent mechanical properties, fatigue resistance, aging resistance and electrical properties in a wide temperature range It has outstanding insulation performance, low production energy consumption and good processing performance, and is widely used in the fields of film, bottle blowing, polyester fiber and engineering plastics.
  • CN2008100377356 discloses that glass fiber-reinforced PET is added with modified nano-reinforcing agents, nucleating agents, toughening agents and other auxiliary agents to obtain high-gloss reinforced and toughened PET nanocomposites; CN2009100402066 strengthens PBT and PMMA composite glass fiber, and adds compatibilizer, nucleating agent, coupling agent and other auxiliary agents to obtain polyester composite material with glossiness exceeding 80; CN2009100571261 reports adding low-viscosity annular Polyester, anti-fiber exposure agent TAF (a kind of synthetic vegetable oil) and other modification aids and nucleating agents prepare no surface floating fiber and good glossy reinforced polyester material; CN2010105902210 discloses the addition of glass fiber reinforced PET/PBT alloy Organic and inorganic composite nucleating agents, and cyclic oligomer functional polyester are used as processing aids to obtain low-warpage materials with good surface gloss and low vertical and horizontal shrinkage; CN2015100
  • the purpose of the present invention is to improve the degree of floating fiber and glossiness of the glass fiber reinforced PBT/PET composite material system, and its preparation method and application.
  • a kind of PBT/PET composite material, by weight, comprises following component:
  • each gram of PBT/PET composite material contains 150-500 micrograms of acetaldehyde.
  • each gram of the PBT/PET composite material contains 200-450 micrograms of acetaldehyde.
  • each gram of the PBT/PET composite material contains 250-400 micrograms of acetaldehyde.
  • the detection method of acetaldehyde content is: use GC-2014 type chromatograph, headspace sampler: column furnace temperature 190 °C, detector temperature 280 °C, injector temperature 250 °C; quantitative method: external standard method, chromatographic column : Carbowax 20M capillary with a length of 60m and a diameter of 0.32mm; to establish a standard curve, inject 0.2, 0.4, 0.6, 0.8, 1.0 ⁇ L of pure acetaldehyde solution (1mg ⁇ mL -1 ) into the well-filled Nitrogen and sealed headspace bottle, put it in the refrigerator for 10 minutes, take it out, put it into the headspace sampler, under the chromatographic conditions, measure the peak area of 5 standard samples, and get the standard of acetaldehyde content Curve; the acetaldehyde content of test sample is measured by external standard method.
  • the flame retardant synergist is selected from melamine cyanurate and/or melamine polyphosphate.
  • the average diameter of the glass fibers is in the range of 10-13 microns.
  • the glossiness of the PBT/PET composite material of the present invention is more than or equal to 78.
  • the preparation method of the PBT/PET composite material of the present invention comprises the following steps: according to the proportion, the components other than the glass fiber are evenly mixed, and then fed into the twin-screw extruder through the main feeding port, and the glass fiber passes through the side Feed and feed, melt and shear to obtain PBT/PET composite material, wherein the maximum temperature range of the screw is 240-255°C, the rotational speed range is 350-550rpm, and the residence time is 20-25s.
  • the factors affecting the decomposition of PET resin from major to minor are: the amount of aluminum diethyl hypophosphite added, the temperature of melting processing, the residence time of melting, the ratio of PET resin to PBT resin, etc.
  • the content of acetaldehyde is mainly adjusted by the addition amount of aluminum diethyl hypophosphite, the temperature of melting processing, and the retention time of melting.
  • the application of the PBT/PET composite material of the present invention is used to prepare electronic component shells and electric appliance shells, and has the advantage of good surface appearance.
  • the present invention utilizes phosphorus-based halogen-free flame retardant (diethylaluminum hypophosphite) to degrade PET so as to produce specific content of acetaldehyde (containing 150-500 micrograms of acetaldehyde per gram of PBT/PET composite material).
  • acetaldehyde containing 150-500 micrograms of acetaldehyde per gram of PBT/PET composite material.
  • PBT resin 1200-211M, Taiwan Changchun Chemical Industry.
  • PET resin FG600, Yizheng chemical fiber.
  • Glass fiber A average diameter 11 microns, ECS11-4.5-534A, Jushi Group;
  • Glass fiber B average diameter 10 microns, HMG436S-10-4.0, Taishan Glass Fiber Co., Ltd.;
  • Glass fiber C average diameter 8 microns, ECS8-03-568H, Jushi Group;
  • Glass fiber D average diameter 14 microns, ECS14-5.0-588, Jushi Group;
  • Aluminum diethyl hypophosphite EXOLIT OP 1230, Clariant;
  • Melamine polyphosphate MPP, Shouguang Weidong Chemical.
  • Talc powder HTPultra5, Ai Haiyi Mi Mining, D 50 is 0.65 ⁇ m.
  • the preparation method of embodiment and comparative example PBT/PET composite material mix the components other than the glass fiber evenly, then feed in the twin-screw extruder through the main feeding port, the glass fiber is fed through the side, melt shear Cut the PBT/PET composite material, wherein, the maximum temperature of the screw is shown in the table, the speed range is 350-550rmp, and the maximum temperature and residence time of the screw are shown in the table.
  • the detection method of acetaldehyde content is: adopt GC-2014 type chromatograph, headspace sampler: column oven temperature 190 °C, detector temperature 280 °C, injector temperature 250 °C; quantitative method: external standard method , chromatographic column: Carbowax 20M capillary with a length of 60m and a diameter of 0.32mm; to establish a standard curve, inject 0.2, 0.4, 0.6, 0.8, 1.0 ⁇ L of pure acetaldehyde solution (1mg ⁇ mL -1 ) into In the headspace bottle filled with nitrogen and sealed, put it in the refrigerator for 10 minutes, take it out, and put it into the headspace sampler. Under the chromatographic conditions, measure the peak area of 5 standard samples to obtain acetaldehyde The standard curve of content; the acetaldehyde content of test sample adopts external standard method to measure.
  • Floating fiber defect use the visual method to observe the floating fiber condition at the same part of the 100 ⁇ 100 ⁇ 2mm square plate: it is divided into 5 grades, 1 grade is no floating fiber; 2 grade is shallow floating fiber, and The number is 1-3; Grade 3 means the floating fibers are shallow and the number is less than 3-5; Grade 4 means the floating fibers protrude more and the number is 5-10; Grade 5 means the floating fibers seriously affect the surface gloss .
  • Table 1 Contents (parts by weight) and test results of each component of the PBT/PET alloy of Examples 1-8
  • the content of acetaldehyde in the composite material can be controlled by adjusting the highest temperature and residence time.
  • the content of acetaldehyde is within the preferred range, the surface gloss is better and the floating fibers are less.
  • Example 3/7/8 it can be seen that by adjusting the content of flame retardant (the main purpose is to adjust the content of aluminum diethyl hypophosphite), the content of acetaldehyde can be significantly changed, and then the glossiness and floating fiber of the alloy can be adjusted.
  • the content of flame retardant the main purpose is to adjust the content of aluminum diethyl hypophosphite
  • the diameter of the glass fiber has a certain influence on the surface gloss and floating fiber, but it hardly affects the content of acetaldehyde. In the preferred diameter range, the surface gloss is higher and the floating fiber is more few.
  • Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6 PBT resin 35 55 45 45 45 45 PET resin 45 10 30 30 30 30 30 aluminum diethyl hypophosphite 11 11 7 18 11 11 Melamine cyanurate 4 4 4 4 4 Glass fiber A 30 30 30 30 30 30 30 30 Maximum temperature, °C 250 250 250 250 235 260 dwell time, s twenty three twenty three twenty three twenty three 19 26 Acetaldehyde content, ⁇ g/g 532 136 142 521 131 550 surface gloss 65.2 58.7 61.7 64.5 55.3 66.4 floating fiber, grade 4 5 4 4 5 4
  • Comparative Example 1 when the PET content is too high, the degradation of PET seriously causes the acetaldehyde content to be greater than 400 ⁇ g/g, which will cause the precipitation of small molecules, increase mold fouling and reduce gloss.
  • Comparative Example 4 it can be seen from Comparative Example 4 that when the content of aluminum diethyl hypophosphite is too high, the content of acetaldehyde is too high, which will lead to a decrease in surface gloss and a deterioration of floating fibers as in Comparative Example 2.

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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)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

本发明公开了一种PBT/PET复合材料，按重量份计，包括以下组分：PBT树脂35-55份；PET树脂15-40份；二乙基次磷酸铝9-16份；阻燃协效剂2-7份；玻璃纤维10-40份；以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有150-500微克乙醛。本发明利用二乙基次磷酸铝对PET降解从而产生特定含量的乙醛，当树脂基体中含有特定量的乙醛时，对复合材料的流动性有改善作用，且极性较强对玻璃纤维的浸润和包覆具有促进作用，减少了浮纤缺陷且提升了表面的光滑程度使得光泽度得到了显著提高。

Description

一种PBT/PET复合材料及其制备方法和应用 技术领域
本发明涉及高分子材料技术领域，特别是涉及一种PBT/PET复合材料及其制备方法和应用。
背景技术
聚对苯二甲酸丁二醇酯PBT因结晶和线性饱和，其具有优良的电性能、机械强度和加工性，改性后的聚酯在电子电气等领域得到广泛的应用。无卤阻燃玻纤增强的PBT常用作冷却风扇扇框扇叶、马达外壳、继电器、连接器等部件，在业界获得大量的认可；聚对苯二甲酸乙二醇酯PET相对PBT而言，具有较高的熔点(Tm)和玻璃化转变温度(Tg)，也是一种线性饱和结晶性聚合物，且在较宽的温度范围内保持优良的机械性能，耐疲劳性能，耐老化性能和电绝缘性能突出，生产能耗低，加工性能好，被广泛应用于薄膜，吹瓶，聚酯纤维和工程塑料等领域。
但因PET分子链柔性较低，结晶速度较慢，存在注塑成型周期长，加玻纤PET材料外观浮纤明显，需要高模温才能获得好的外观效果等不足，众多元器件作为外观件对其外观的要求苛刻，如低浮纤、高光泽等，限制了其在工程塑料领域里的应用。
公开报道改性聚酯实现高光泽的方法众多，CN2008100377356公开了将玻纤增强的PET加入改性纳米增强剂，成核剂，增韧剂等助剂获得高光泽增强增韧PET纳米复合材料；CN2009100402066将PBT与PMMA复合玻纤增强，加入相容剂、成核剂、偶联剂等助剂得到光泽度超过80聚酯复合材料；CN2009100571261报道在玻纤增强的PET材料中加入低粘环状聚酯，防纤维外露剂TAF(一种合成植物油)等改性助剂和成核剂制备无表面浮纤和光泽度好的增强聚酯材料；CN2010105902210公开了玻纤增强的PET/PBT合金加入有机和无机的复合成核剂，以及环状低聚物功能聚酯作为加工助剂获得表面光泽度良好，纵横向收缩率比较低的低翘曲材料；CN2015100566108报道玻纤增强的PBT/PP合金，加入线型低密度聚乙烯作为表面光亮剂，相容剂和增粘的聚乙烯醇缩丁醛作为PBT结晶抑制剂来获得光泽度大于83的玻纤增强复合材料；CN2016111751427公开了PBT/PET玻纤增强复合材料通过加入高流动性的聚丁二酸丁二醇酯(PBS)树脂改善树脂对玻纤的润湿与包覆以改善浮纤，获得高光泽度效果；CN2018105031305报道了玻纤增强聚酰胺通过加入纳米填料和超支化聚酯作为流动改性剂所得聚酰胺组合物具有较高的光泽度和较少的浮纤。但是上述方案都是添加其他助剂来提升表面光泽度，这会在一定程度上改变复合材料的其他性能。
发明内容
本发明的目的在于，改善玻纤增强PBT/PET复合材料体系的浮纤程度并且提高光泽度，及其制备方法和应用。
本发明是通过以下技术方案实现的：
一种PBT/PET复合材料，按重量份计，包括以下组分：
Figure PCTCN2022139529-appb-000001
以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有150-500微克乙醛。
优选的，以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有200-450微克乙醛。
更优选的，以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有250-400微克乙醛。
乙醛含量的检测方法为：采用GC-2014型色谱仪，顶空进样器：柱炉温度190℃，检测器温度280℃，进样器温度250℃；定量方法：外标法，色谱柱：Carbowax 20M毛细管长60m，直径0.32mm；标准曲线建立，分别用1μL的进样针准确注射0.2、0.4、0.6、0.8、1.0μL的纯乙醛溶液(1mg·mL -1)到已充好氮气并封好口的顶空瓶中，放入冰箱冷冻10min后取出，放入顶空进样器内，在该色谱条件下，对5个标准样品测定其峰面积，得到乙醛含量的标准曲线；测试样品的乙醛含量采用外标法进行测量。
所述的阻燃协效剂选自三聚氰胺氰尿酸盐和/或三聚氰胺聚磷酸盐。
所述的玻璃纤维的平均直径范围是10-13微米。
为了进一步提升表面光泽度，按重量份计，还包括0-2份D50＝0.1-5微米的滑石粉。
本发明的PBT/PET复合材料的光泽度≥78。
本发明的PBT/PET复合材料的制备方法，包括以下步骤：按照配比，将玻璃纤维之外的组分混合均匀，再通过主喂料口喂入双螺杆挤出机中，玻璃纤维通过侧喂喂入，熔融剪切得到PBT/PET复合材料，其中，螺杆最高温度范围是240-255℃，转速范围是350-550rpm、停留时间为20-25s。
影响PET树脂的分解因素由主至次依次为：二乙基次磷酸铝的添加量、熔融加工的温 度、熔融的停留时间、PET树脂与PBT树脂的比例等。本发明具体实施方式中主要通过二乙基次磷酸铝的添加量、熔融加工的温度、熔融的保留时间来调节乙醛的含量。
本发明的PBT/PET复合材料的应用，用于制备电子元器件外壳、电器外壳，具有表面外观好的优点。
本发明具有如下有益效果：
本发明利用磷系无卤阻燃剂(二乙基次磷酸铝)对PET降解从而产生特定含量的乙醛(每克PBT/PET复合材料中含有150-500微克乙醛)，当树脂基体中含有特定量的乙醛时，对复合材料的流动性有改善作用，且极性较强对玻璃纤维的浸润和包覆具有促进作用，减少了浮纤缺陷且提升了表面的光滑程度使得光泽度得到了显著提高。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例和对比例所用原材料来源如下：
PBT树脂：1200-211M，台湾长春化工。
PET树脂：FG600，仪征化纤。
玻璃纤维A：平均直径11微米，ECS11-4.5-534A，巨石集团；
玻璃纤维B：平均直径10微米，HMG436S-10-4.0，泰山玻璃纤维有限公司；
玻璃纤维C：平均直径8微米，ECS8-03-568H，巨石集团；
玻璃纤维D：平均直径14微米，ECS14-5.0-588，巨石集团；
二乙基次磷酸铝：EXOLIT OP 1230，科莱恩；
三聚氰胺氰尿酸盐：MCA，四川精细化工；
三聚氰胺聚磷酸盐：MPP，寿光卫东化工。
滑石粉：HTPultra5,艾海意米矿业，D 50为0.65μm。
实施例和对比例PBT/PET复合材料的制备方法：将玻璃纤维之外的组分混合均匀，再通过主喂料口喂入双螺杆挤出机中，玻璃纤维通过侧喂喂入，熔融剪切得到PBT/PET复合材料，其中，螺杆最高温度请见表格，转速范围是350-550rmp，螺杆的最高温度、停留时间见表格。
各项测试方法：
(1)乙醛含量的检测方法为：采用GC-2014型色谱仪，顶空进样器：柱炉温度190℃，检测器温度280℃，进样器温度250℃；定量方法：外标法，色谱柱：Carbowax 20M毛细管长60m，直径0.32mm；标准曲线建立，分别用1μL的进样针准确注射0.2、0.4、0.6、0.8、1.0μL的纯乙醛溶液(1mg·mL -1)到已充好氮气并封好口的顶空瓶中，放入冰箱冷冻10min后取出，放入顶空进样器内，在该色谱条件下，对5个标准样品测定其峰面积，得到乙醛含量的标准曲线；测试样品的乙醛含量采用外标法进行测量。
(2)表面光泽度：按ASTM D2457-2013，测试选用60°角，在相同的注塑工艺参数下注塑测试试样，试样尺寸为100×100×2mm。
(3)浮纤缺陷：采用目视的方法，在100×100×2mm方板的相同部位观察浮纤状况：分为5级，1级为无浮纤；2级为浮纤较浅、并且数量1-3根；3级为浮纤较浅、并且数量少于3-5根；4级为浮纤突出较多、并且数量5-10根；5级为浮纤严重影响了表面光泽度。
表1：实施例1-8 PBT/PET合金各组分含量(重量份)及测试结果
Figure PCTCN2022139529-appb-000002
由实施例1-6可知，通过调整最高温以及停留时间，能够控制复合材料中乙醛的含量，当乙醛含量在优选范围内时，表面光泽度更好，浮纤更少。
由实施例3/7/8可知，通过调整阻燃剂的含量(主要目的是调整二乙基次磷酸铝含量)，能够显著改变乙醛含量，进而调整合金的光泽度与浮纤。
表2：实施例9-15 PBT/PET合金各组分含量(重量份)及测试结果
Figure PCTCN2022139529-appb-000003
Figure PCTCN2022139529-appb-000004
由实施例3/9/10可知，PBT/PET树脂的不同含量也显著影响合金中的乙醛含量。
由实施例3、12-14可知，玻璃纤维的直径对于表面光泽度与浮纤具有一定的影响，但几乎不影响乙醛的含量，在优选的直径范围内，表面光泽度更高浮纤更少。
表3：对比例PBT/PET合金各组分含量(重量份)及测试结果
  对比例1 对比例2 对比例3 对比例4 对比例5 对比例6
PBT树脂 35 55 45 45 45 45
PET树脂 45 10 30 30 30 30
二乙基次磷酸铝 11 11 7 18 11 11
三聚氰胺氰尿酸盐 4 4 4 4 4 4
玻璃纤维A 30 30 30 30 30 30
最高温，℃ 250 250 250 250 235 260
停留时间，s 23 23 23 23 19 26
乙醛含量，微克/克 532 136 142 521 131 550
表面光泽度 65.2 58.7 61.7 64.5 55.3 66.4
浮纤，级 4 5 4 4 5 4
由对比例1可知，当PET含量过高时，PET降解严重导致乙醛含量大于400微克/克，这样会使得小分子析出，增加模垢和降低光泽度。
由对比例2可知，当PET含量过低时，可降解的PET较少，乙醛含量较低，对于玻纤的浸润效果不佳，使得表面光泽度与浮纤较差。
由对比例3可知，当二乙基次磷酸铝含量过低，无法有效降解PET树脂导致乙醛含量过低，对于玻纤的浸润效果不佳，表面光泽度与浮纤较差。
由对比例4可知，当二乙基次磷酸铝含量过高时，乙醛含量过高，同对比例2会导致表面光泽度的下降以及浮纤的变差。
由对比例5可知，当加工温度低、停留时间不足时，也无法充分降解PET树脂以达到150-500微克/克的乙醛含量，合金的表面光泽度低、浮纤明显。
由对比例6可知，当加工温度过高、停留时间过长时，乙醛含量过高，也使得光泽度的下降以及浮纤的变差。

Claims (10)

  1. 一种PBT/PET复合材料，其特征在于，按重量份计，包括以下组分：
    Figure PCTCN2022139529-appb-100001
    以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有150-500微克乙醛。
  2. 根据权利要求将1所述的PBT/PET复合材料，其特征在于，以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有200-450微克乙醛。
  3. 根据权利要求将2所述的PBT/PET复合材料，其特征在于，以PBT/PET复合材料的总重量计，每克PBT/PET复合材料中含有250-400微克乙醛。
  4. 根据权利要求1-3任一项所述的PBT/PET复合材料，其特征在于，乙醛含量的检测方法为：采用GC-2014型色谱仪，顶空进样器：柱炉温度190℃，检测器温度280℃，进样器温度250℃；定量方法：外标法，色谱柱：Carbowax 20M毛细管长60m，直径0.32mm；标准曲线建立，分别用1μL的进样针准确注射0.2、0.4、0.6、0.8、1.0μL的纯乙醛溶液(1mg·mL -1)到已充好氮气并封好口的顶空瓶中，放入冰箱冷冻10min后取出，放入顶空进样器内，在该色谱条件下，对5个标准样品测定其峰面积，得到乙醛含量的标准曲线；测试样品的乙醛含量采用外标法进行测量。
  5. 根据权利要求将1所述的PBT/PET复合材料，其特征在于，所述的阻燃协效剂选自三聚氰胺氰尿酸盐和/或三聚氰胺聚磷酸盐。
  6. 根据权利要求将1所述的PBT/PET复合材料，其特征在于，所述的玻璃纤维的平均直径范围是10-13微米。
  7. 根据权利要求将1所述的PBT/PET复合材料，其特征在于，按重量份计，还包括0-2份D50＝0.1-5微米的滑石粉。
  8. 根据权利要求1-7任一项所述的PBT/PET复合材料，其特征在于，所述的PBT/PET复合材料的光泽度≥78。
  9. 权利要求1-8任一项所述PBT/PET复合材料的制备方法，其特征在于，包括以下步骤：按照配比，将玻璃纤维之外的组分混合均匀，再通过主喂料口喂入双螺杆挤出机中，玻璃纤维通过侧喂喂入，熔融剪切得到PBT/PET复合材料，其中，螺杆最高温度范围是240-255℃，转速范围是350-550rmp、停留时间为20-25s。
  10. 权利要求1-8任一项所述PBT/PET复合材料的应用，其特征在于，用于制备电子元器件外壳、电器外壳。
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