WO2020134845A1 - 一种阻燃尼龙复合材料及其应用 - Google Patents

一种阻燃尼龙复合材料及其应用 Download PDF

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WO2020134845A1
WO2020134845A1 PCT/CN2019/121747 CN2019121747W WO2020134845A1 WO 2020134845 A1 WO2020134845 A1 WO 2020134845A1 CN 2019121747 W CN2019121747 W CN 2019121747W WO 2020134845 A1 WO2020134845 A1 WO 2020134845A1
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flame
composite material
parts
retardant nylon
nylon composite
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PCT/CN2019/121747
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English (en)
French (fr)
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郑一泉
金雪峰
冯德才
丁超
胡泽宇
何勇
黄险波
叶南飚
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金发科技股份有限公司
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Priority to US17/418,854 priority Critical patent/US20220073741A1/en
Priority to EP19901740.1A priority patent/EP3892684A4/en
Publication of WO2020134845A1 publication Critical patent/WO2020134845A1/zh
Priority to AU2020101367A priority patent/AU2020101367A4/en

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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
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/13—Phenols; Phenolates
    • 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
    • C08K3/02—Elements
    • 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
    • C08K3/40—Glass
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/05—Alcohols; Metal alcoholates
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/07—Aldehydes; Ketones
    • C08K5/08—Quinones
    • 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
    • C08K3/02—Elements
    • C08K2003/026—Phosphorus
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets

Definitions

  • the invention relates to the technical field of engineering plastics, in particular to a flame retardant nylon composite material and its application.
  • Red phosphorus flame retardant nylon has the advantages of excellent electrical properties (CTI, electrical breakdown strength), high flame retardant efficiency and low price, and is widely used in electrical and electronic industries.
  • CTI electrical breakdown strength
  • Red phosphorus is a very effective flame retardant and can be used in oxygen-containing polymers, but because red phosphorus will react with water vapor in the atmosphere to produce odorous and toxic phosphine, therefore, it needs to be stabilized and coated in industry .
  • Patent US5434209 discloses a method for improving red phosphorus precipitation, which uses bisphenol Z or bisphenol S, which can reduce the precipitation of phosphine to a lower level.
  • Patent US6645625 discloses a method for improving the precipitation of red phosphorus. Using silver or tin oxide, the precipitation of phosphine can be reduced to less than 0.01 mg/g, but the use of metal elements will affect the electrical properties of the material.
  • Patent US8883904 discloses a method for improving the precipitation of red phosphorus. The mixture of silver and zinc oxide can reduce the precipitation of phosphorus to 15ug/g, but the use of the same metal elements will affect the electrical properties of the material.
  • Patent CN93101597 discloses a method for improving phosphorus precipitation. Using zinc oxide and zinc borate, the phosphorus precipitation of red phosphorus flame retardant nylon system can be reduced to a lower level, but zinc borate will affect the mechanical properties.
  • the present invention has unexpectedly discovered through research that adding a small amount of phenols to the flame-retardant nylon composite material can effectively suppress the precipitation of phosphorus while maintaining good electrical properties.
  • the purpose of the present invention is to provide a flame-retardant nylon composite material, which can effectively suppress the precipitation of phosphorus by adding phenols, while maintaining good electrical properties.
  • a flame retardant nylon composite material including the following components:
  • Phenolic substances 0.01 parts to 2 parts.
  • the phenolic substance is one or a mixture of 2,5-di-tert-butylhydroquinone, o-methylhydroquinone or 2-methylphenol.
  • the present invention can effectively suppress the precipitation of phosphorus while maintaining good electrical properties.
  • the amount of phenols is based on the total weight of the nylon composite material. It is better to add 0.01-2 parts. If the amount is too small, the effect of suppressing phosphorus precipitation is not obvious. If the amount is too much, precipitation will affect the appearance of the product.
  • the nylon resin is one or a mixture of PA66, PA6/6,10 or PA6,6/6.
  • Red phosphorus is used as a flame retardant in composite materials.
  • Red phosphorus powder is preferably used, with an average diameter not exceeding 300 ⁇ m, and a preferred particle size of 1-100 ⁇ m.
  • the flame-retardant nylon composite material is characterized in that, in terms of parts by weight, it further includes 8 parts to 55 parts of glass fiber, and the glass fiber uses at least one type from the following group Glass fiber: E glass, H glass, R, S glass, D glass, C glass or quartz glass, it is particularly preferable to use glass fiber made of E glass.
  • the flame-retardant nylon composite material of the present invention in terms of parts by weight, also includes lubricants, nucleating agents, antistatic agents, etc., with a weight content of 1 part to 5 parts.
  • the preparation method of the flame-retardant nylon composite material provided by the present invention can be obtained by weighing each raw material according to a certain ratio, premixing in a high-mixer to obtain a premix, and then putting the premix into a twin screw extruder Melting and mixing in the machine, and extrusion granulation to obtain flame retardant nylon composite material; wherein the screw length-diameter ratio of the twin screw extruder is 40-48:1, the barrel temperature is 250-270°C, and the screw speed is 200-550rpm.
  • the invention also provides the application of the flame-retardant nylon composite material in electronic appliances.
  • the invention also provides the application of phenols in improving the precipitation of red phosphorus in flame retardant nylon composite materials.
  • the phenols are 2,5-di-tert-butylhydroquinone, o-methylhydroquinone or 2 -A mixture of one or more of methylphenol. Based on the total weight of the flame-retardant nylon composite material, the added amount of the phenolic substance is 0.01-2 parts.
  • the present invention has the following beneficial effects:
  • the invention can effectively suppress the precipitation of phosphorus by adding a small amount of phenols to the red phosphorus flame retardant nylon composite material, can reduce the precipitation of phosphine to 30ppm or less, while maintaining good electrical performance, suitable for use Used in the fields of connectors and contactors in electronic appliances.
  • PA66-a PA66 50FWFS, industrial grade, ASCEND company;
  • PA66-b 21ZLV, industrial grade, ASCEND company
  • Red phosphorus RPM440B, average particle size 40 ⁇ m, Zhonglan Chenguang Chemical Research and Design Institute Co., Ltd.;
  • O-Methylhydroquinone Aladdin reagent (Shanghai) Co., Ltd.;
  • Silver powder purity 99.99%, particle size less than 0.1um; Aladdin reagent (Shanghai) Co., Ltd.;
  • Zinc oxide purity 99.99%, metals basis, Aladdin reagent (Shanghai) Co., Ltd.;
  • Zinc borate anhydrous zinc borate, particle size 20-30um, Aladdin reagent (Shanghai) Co., Ltd.;
  • Glass fiber ECS301HP-3, Chongqing International Composite Materials Co., Ltd.
  • Phosphorus precipitation between a platinum electrode of a specified size, a certain voltage is applied and a specified height (30mm) of a contaminated liquid (0.1% ammonium chloride) is dripped at a fixed height (30mm) at regular intervals (ppm): Place deionized water, 2g silver flakes, 2g copper flakes, and 6g red phosphorus particles in an 80-degree oven for 3 days, then wash the copper flakes and silver flakes with 100ml of 0.1mol/L hydrochloric acid solution. -AES determination of phosphorus content in hydrochloric acid solution.
  • the composite materials prepared in the above examples and comparative examples are first injected into standard samples for testing according to the standard size, and each performance test is performed; the performance test data of the samples of each example is shown in Table 1.
  • Example 5 Example 6
  • Example 7 Example 8
  • PA66-b 60 60 60 43 RPM440B 9 12 13 7
  • O-methyl hydroquinone A
  • A 0.2 2,5-di-tert-butyl hydroquinone 1.2 1 1.5
  • Glass fiber ECS301HP-3 25 25 50 CTI(V) 400 375 350
  • the present invention can effectively suppress the precipitation of phosphorus by adding a small amount of phenols to the red phosphorus flame retardant nylon composite material, and can reduce the precipitation of phosphine to 30 ppm or less. Can maintain good electrical performance.

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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

本发明公开了一种阻燃尼龙复合材料及其应用，包括组分：尼龙树脂55份-80份；红磷1份-30份；酚类物质0.01份-2份。本发明通过在红磷阻燃尼龙复合材料中加入少量的酚类物质，可以有效的抑制磷析出，可以将磷化氢的析出量降低到30ppm或以下，同时能保持良好的电性能，适合用于电子电器中的连接器、接触器等领域。

Description

一种阻燃尼龙复合材料及其应用 技术领域
本发明涉及工程塑料技术领域，具体涉及一种阻燃尼龙复合材料及其应用。
背景技术
红磷阻燃尼龙具有电性能优异(CTI，电击穿强度)，阻燃效率高以及价格低廉等优势，广泛应用于电子电气等行业。红磷是非常有效的阻燃剂，可用于含氧聚合物，但由于红磷会与大气中的水汽反应生成有气味且有毒的磷化氢，因此，工业上需要作稳定化处理和包覆。
专利US5434209公开了一种改善红磷析出的方法，其采用双酚Z或双酚S，可以将磷化氢的析出量降低到较低的水平。专利US6645625公开了一种改善红磷析出的方法，采用银或氧化锡，可以将磷化氢的析出量降低到0.01mg/g以下，但是金属元素的使用会影响材料的电气性能。专利US8883904公开了一种改善红磷析出的方法，采用银和氧化锌的混合物，可以将磷析出量降低到15ug/g，但是同样金属元素的使用会影响材料的电气性能。专利CN93101597公开了一种改善磷析出的方法，采用氧化锌和硼酸锌，可以使红磷阻燃尼龙体系的磷析出降低到较低的水平，但是硼酸锌等会影响力学性能。
本发明通过研究意外的发现，在阻燃尼龙复合材料添加少量的酚类物质，可以有效的抑制磷析出，同时能保持良好的电性能。
发明内容
本发明的目的在于提供一种阻燃尼龙复合材料，通过加入酚类物质，可以有效的抑制磷析出，同时能保持良好的电性能。
本发明是通过以下技术方案实现的：
一种阻燃尼龙复合材料，按重量份数计，包括以下组分：
尼龙树脂  55份-80份；
红磷      1份-30份；
酚类物质  0.01份-2份。
优选的，所述酚类物质为2,5-二特丁基对苯二酚、邻甲基对苯二酚或2-甲基苯酚中的一种或几种的混合。本发明通过在复合材料中引入少量的酚类物质，可以有效的抑制磷析出，同时能保持良好的电性能。酚类物质的量以尼龙复合材料的总重量份数计，加入0.01-2份为 宜，如果添加量过少，抑制磷析出的效果不明显，如果添加量过多，会析出影响产品外观。
优选的，所述尼龙树脂为PA66、PA6/6,10或PA6,6/6的一种或几种的混合。
红磷作为阻燃剂用于复合材料中，优选使用红磷粉，平均直径不超过300μm，优选粒径为1-100μm。
作为进一步优选的技术方案，所述的阻燃尼龙复合材料，其特征在于，按重量份数计，还包括8份-55份玻璃纤维，所述玻璃纤维是使用至少一种类型的来自下组的玻璃纤维：E玻璃、H玻璃、R,S玻璃、D玻璃、C玻璃或石英玻璃，特别优选的是使用由E玻璃制成的玻璃纤维。
根据实际性能需要，本发明所述阻燃尼龙复合材料，按重量份数计，还包括润滑剂、成核剂、抗静电剂等，重量含量在1份-5份。
本发明所提供的阻燃尼龙复合材料的制备方法，可通过如下方法得到：按照一定比例称取各原料，在高混机中进行预混合得到预混料，然后将预混物投入双螺杆挤出机中进行熔融混合，并挤出造粒，得到阻燃尼龙复合材料；其中双螺杆挤出机的螺杆长径比为40-48:1，螺筒温度为250-270℃，螺杆转速为200-550rpm。
本发明还提供了上述阻燃尼龙复合材料在电子电器中的应用。
本发明还提供了酚类物质在改善阻燃尼龙复合材料红磷析出中的应用，所述酚类物质为2,5-二特丁基对苯二酚、邻甲基对苯二酚或2-甲基苯酚中的一种或几种的混合。以阻燃尼龙复合材料的总重量计，所述酚类物质的加入量为0.01-2份。
与现有技术相比，本发明具有如下有益效果：
本发明通过在红磷阻燃尼龙复合材料中加入少量的酚类物质，可以有效的抑制磷析出，可以将磷化氢的析出量降低到30ppm或以下，同时能保持良好的电性能，适合用于电子电器中的连接器、接触器等领域。
具体实施方式
下面给出实施例以对本发明进行具体的描述，但不限于此。
现对实施例及对比例所用的原材料做如下说明，但不限于这些材料：
PA66-a：PA66 50FWFS，工业级，ASCEND公司；
PA66-b:21ZLV,工业级，ASCEND公司；
红磷：RPM440B，平均粒径40μm，中蓝晨光化工研究设计院有限公司；
2,5-二叔丁基对苯二酚：阿拉丁试剂(上海)有限公司；
邻甲基对苯二酚：阿拉丁试剂(上海)有限公司；
银粉：纯度99.99％，粒径小于0.1um；阿拉丁试剂(上海)有限公司；
氧化锌：纯度99.99％，metals basis，阿拉丁试剂(上海)有限公司；
硼酸锌：无水硼酸锌，粒径20-30um，阿拉丁试剂(上海)有限公司；
玻璃纤维：ECS301HP-3，重庆国际复合材料有限公司。
性能测试方法：
相比起痕指数(CTI)：按IEC60112-2003标准测试。
磷析出量：在规定尺寸的铂电极之间，施加某一电压并定时(30s)定高度(30mm)滴下规定液滴体积的污染液体(0.1％的氯化铵)磷析出量(ppm)：将去离子水，2g银片和2g铜片以及6g红磷粒分别置于80度的烘箱中，放置3天，然后用100ml的0.1mol/L的盐酸溶液洗涤铜片和银片，用ICP-AES测定盐酸溶液中的磷含量。
实施例1-8和对比例1-3：
按表1配比称取各原料，在高混机中进行预混合得到预混料，然后将预混物投入双螺杆挤出机中进行熔融混合，并挤出造粒，得到阻燃尼龙复合材料；其中双螺杆挤出机的螺杆长径比为40-48:1，螺筒温度为250-270℃，螺杆转速为200-550rpm。
将上述各实施例和对比例所制得的复合材料先按标准尺寸注塑成测试用的标准样条，进行各性能测试；各例试样的性能测试数据见表1所示。
表1各实施例及对比例中各组份的具体配比(重量份)
Figure PCTCN2019121747-appb-000001
续表1
  实施例5 实施例6 实施例7 实施例8
PA66-b 60 60 60 43
RPM440B 9 12 13 7
邻甲基对苯二酚       0.2
2,5-二叔丁基对苯二酚 1.2 1 1.5 0.2
玻璃纤维ECS301HP-3 30 25 25 50
CTI(V) 400 375 350 300
磷析出量(ppm) 29 16 23 30
由表2的结果可以看出，本发明通过在红磷阻燃尼龙复合材料中加入少量的酚类物质，可以有效的抑制磷析出，可以将磷化氢的析出量降低到30ppm或以下，同时能保持良好的电性能。

Claims (10)

  1. 一种阻燃尼龙复合材料，其特征在于，按重量份数计，包括以下组分：
    尼龙树脂                  55份-80份；
    红磷                      1份-30份；
    酚类物质                  0.01份-2份。
  2. 根据权利要求1所述的阻燃尼龙复合材料，其特征在于，所述酚类物质为2,5-二特丁基对苯二酚、邻甲基对苯二酚或2-甲基苯酚中的一种或几种的混合。
  3. 根据权利要求1所述的阻燃尼龙复合材料，其特征在于，所述尼龙树脂为PA66、PA6/6,10或PA6,6/6的一种或几种的混合。
  4. 根据权利要求1所述的阻燃尼龙复合材料，其特征在于，所述红磷为红磷粉，平均直径不超过300μm，优选粒径为1-100μm。
  5. 根据权利要求1所述的阻燃尼龙复合材料，其特征在于，按重量份数计，还包括8份-55份玻璃纤维，所述玻璃纤维是使用至少一种类型的来自下组的玻璃纤维：E玻璃、H玻璃、R,S玻璃、D玻璃、C玻璃或石英玻璃，特别优选的是使用由E玻璃制成的玻璃纤维。
  6. 根据权利要求1所述的阻燃尼龙复合材料，其特征在于，按重量份数计，还包括1-5份的成核剂、抗静电剂或润滑剂中的一种或几种。
  7. 根据权利要求1-6任一项所述的阻燃尼龙复合材料在电子电器中的应用。
  8. 酚类物质在改善阻燃尼龙复合材料红磷析出中的应用。
  9. 根据权利要求8所述的应用，其特征在于，所述酚类物质为2,5-二特丁基对苯二酚、邻甲基对苯二酚或2-甲基苯酚中的一种或几种的混合。
  10. 根据权利要求8所述的应用，其特征在于，以阻燃尼龙复合材料的总重量计，所述酚类物质的加入量为0.01-2份。
PCT/CN2019/121747 2018-12-28 2019-11-28 一种阻燃尼龙复合材料及其应用 WO2020134845A1 (zh)

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CN115093701B (zh) * 2022-07-15 2023-08-11 华润化学材料科技股份有限公司 一种高阻隔尼龙及其制备方法和应用

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EP3892684A4 (en) 2022-03-16
CN109777094A (zh) 2019-05-21

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