WO2017118222A1 - 一种军用储油袋tpu复合材料及其制备方法 - Google Patents

一种军用储油袋tpu复合材料及其制备方法 Download PDF

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WO2017118222A1
WO2017118222A1 PCT/CN2016/106176 CN2016106176W WO2017118222A1 WO 2017118222 A1 WO2017118222 A1 WO 2017118222A1 CN 2016106176 W CN2016106176 W CN 2016106176W WO 2017118222 A1 WO2017118222 A1 WO 2017118222A1
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oil storage
tpu
composite material
storage bag
parts
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French (fr)
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郑玉婴
欧忠星
林锦贤
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福州大学
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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
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • 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
    • C08L2201/04—Antistatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Definitions

  • the invention belongs to the technical field of preparation of polymer composite film, and particularly relates to a military oil storage bag TPU composite material and a preparation method thereof.
  • thermoplastic polyurethane elastomer is a (AB)n-type block linear polymer which is composed of a diisocyanate, a polyol and a short-chain diol and which is heated and can be dissolved in a solvent.
  • Polyurethane is a polymer material with a wide range of applications, mainly used in automotive, construction, paving materials, mining, mining, electronics and aerospace. In recent years, polyurethane grouting materials, which are one of the important chemical strengthening materials, have also developed rapidly. And people have turned their attention to TPU water storage bags, TPU military oil storage bags, TPU wading products.
  • TPU as a military oil storage bag
  • soft oil bags have the advantages of light weight, small size, no rust, convenient loading and unloading, and easy to deploy and withdraw. They are widely used in the battlefield to store bulk oil.
  • soft oil tanks can also be placed on vehicles, ships and aircraft as oil containers.
  • Some soft oil tanks can also be used for air transport, airdrop, helicopter lift, water haulage and underwater storage of oil. It can replace traditional iron tanks or fuel tanks in many fields such as oil storage and pipeline repair, becoming a new way to store and transport liquids.
  • the polyurethane material itself has a high surface resistance, and it is easy to generate static charge accumulation during use, which is an important hidden danger of fire, explosion and other safety accidents.
  • the object of the present invention is to provide a military oil storage bag TPU composite material and a preparation method thereof according to the deficiencies and defects in the prior art.
  • the composite material prepared by the method of the invention has excellent mechanical and antistatic properties, flame retardant property and anti-aging and anti-yellowing property, safety and environmental protection, and thermal stability can be further improved, and is particularly suitable for preparing a storage water storage bag film. Materials with a wide range of social and economic benefits as well as strategic value.
  • the present invention adopts the following technical solutions:
  • TPU oil storage bag is composed of the following components by weight: 100 parts of polyurethane elastomer (TPU), 10-40 parts of nylon 6 (PA6), EVA-g- MAH 5-25 parts, antistatic agent 5-10 parts, modified magnesium hydroxide 5-15 parts, antioxidant 0.1-0.5 parts, combined anti-aging anti-yello agent 1-2.5 parts;
  • the combined anti-aging anti-yellowing agent is composed of an antioxidant 1010, a UV absorber UV-232 and a hindered amine light stabilizer UV-622, and the mass ratio thereof is 2:3:3.
  • the antioxidant is an antioxidant 168.
  • the antistatic agent is ATO powder, wherein the mass ratio of SnO 2 and Sb 2 O 3 is 90:10.
  • the modified magnesium hydroxide is prepared by adding magnesium hydroxide particles, 3-methacryloxypropyltrimethoxysilane, cyclohexane and n-propylamine to a three-necked flask, stirring at room temperature for 30 minutes, and then The temperature was raised to 60 ° C and stirred for 30 min; after the reaction was completed, the suspension was placed in a rotary evaporator, and then rotary evaporated under vacuum at 60 ° C for 10 min, then heated to 95 ° C under vacuum for 40 min; finally, the modified hydrogen peroxide The magnesium was dried in a vacuum oven at 80 ° C for 24 h, and after grinding, modified magnesium hydroxide particles were obtained.
  • the EVA-g-MAH is prepared by dissolving azobisisobutyronitrile and dicumyl peroxide in an acetone solution, adding an ethylene-vinyl acetate copolymer (EVA), and drying with maleic anhydride. (MAH) was poured into a twin-screw extruder together, and after extrusion granulation, it was purified by suction filtration to obtain EVA-g-MAH.
  • a method for preparing a military oil storage bag TPU composite material according to any one of the above claims: drying polyurethane elastomer, nylon 6, EVA-g-MAH, antistatic agent, modified magnesium hydroxide, antioxidant After mixing and anti-aging anti-yellowing agent, the mixture is poured into a twin-screw extruder for extrusion granulation, and after drying, a military oil storage bag TPU composite material is obtained by calendering.
  • the preparation method of the military oil storage bag TPU composite material in the twin-screw extruder, during the extrusion granulation process, the temperature of the melt section of the cylinder is controlled at 225 ° C - 230 ° C; the screw speed of the extruder is 300 r / min.
  • the military oil storage bag TPU composite film prepared by the invention can greatly improve the mechanical properties of the TPU material, and the presence of the ATO powder causes the volume resistivity of the composite material to drop sharply by nearly 7 orders of magnitude, achieving an antistatic effect.
  • the limiting oxygen index (LOI) increased from 19.5 to 27.8, and the yellowing level reached 4.1 after 8 hours of exposure to ultraviolet light;
  • the invention combines TPU and PA6 to obtain an alloy with excellent comprehensive performance by adding a compatibilizing agent to reduce the cost of simply using TPU material, and the prepared military oil storage bag TPU composite material has good antistatic property. , flame retardant properties, and at the same time, through the synergistic effect of anti-aging anti-yellowing agent, improve the defects of TPU easy to aging and yellowing;
  • the TPU composite film prepared by the invention is safe and environmentally friendly, and is especially suitable for preparing film materials for water storage and oil storage bags; meanwhile, the invention is suitable for the needs of the market today, and the preparation method is scientific and reasonable, the process is simple, and the operation is strong. It greatly increases the added value of TPU products and expands its application range, with broad market prospects and significant social benefits.
  • TPU alloy composite particles are prepared by extrusion granulation according to the following formulation ratio and component requirements.
  • TPU resin 100 parts
  • PA6 resin 20 parts
  • ATO powder 5 parts;
  • Combination anti-aging anti-yellowing agent 1 part;
  • Antioxidant 168 0.2 parts
  • Modified magnesium hydroxide 5 parts;
  • TPU alloy composite particles are prepared by extrusion granulation according to the following formulation ratio and component requirements.
  • TPU resin 100 parts
  • PA6 resin 30 parts
  • ATO powder 7 parts
  • Combination anti-aging anti-yellowing agent 1.7 parts
  • Antioxidant 168 0.2 parts
  • Modified magnesium hydroxide 10 parts;
  • TPU alloy composite particles are prepared by extrusion granulation according to the following formulation ratio and component requirements.
  • TPU resin 100 parts
  • PA6 resin 50 parts
  • ATO powder 10 parts;
  • Combination anti-aging anti-yellowing agent 2.5 parts;
  • Antioxidant 168 0.2 parts
  • Modified magnesium hydroxide 15 parts;
  • Example 2 Example 3 Tensile strength MPa 28.3 44.65 52.74 49.28 Bending strength MPa 28.02 25.75 24.93 21.05 Notched impact strength KJ/m 2 23.08 107.38 111.65 119.96 Elongation at break % 364.52 303.13 317.39 332.65 Volume resistivity ⁇ cm >10 12 8.9 ⁇ 10 8 5.6 ⁇ 10 7 2.3 ⁇ 10 8 Limiting oxygen index 19.5 25.3 27.8 27.6 Yellowing grade 2.0 3.5 3.8 4.1
  • the composite material film provided by the invention is suitable for preparing fields of TPU medical mattress, TPU biogas storage bag, TPU wading product, TPU water storage oil storage bag and the like, which have high requirements for material barrier and antistatic 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)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

本发明公开了一种军用储油袋TPU复合材料的制备方法，以热塑性聚氨酯弹性体(TPU)及尼龙6(PA6)为基体，采用自制相容剂(EVA-g-MAH)降低TPU与PA6两相间的界面张力，改善体系的相容性，并以ATO粉为抗静电剂，改性MH为阻燃剂，组合抗老抗黄剂经熔融共混后挤出造粒，并压延成型制得性能优异的储油袋用TPU复合材料。本发明通过加入相容剂使得TPU与PA6共混制取综合性能优良的合金来达到降低单纯使用TPU材料的成本，同时所制备的军用储油袋TPU复合材料拥有良好的抗静电性能、阻燃性能，同时通过组合抗老抗黄剂的协同作用，改善TPU易老化易黄变的缺陷。

Description

一种军用储油袋TPU复合材料及其制备方法 技术领域
本发明属于高分子复合薄膜制备技术领域，具体涉及一种军用储油袋TPU复合材料及其制备方法。
背景技术
热塑性聚氨酯弹性体(TPU)是由二异氰酸酯、多元醇及短链二元醇所组成的一种加热可以塑化、溶剂可以溶解的(AB)n型嵌段线性聚合物。聚氨酯是一种具有广泛用途的高分子材料，主要用于汽车、建筑、铺装材料、矿山、开采、电子和航天等方面。近年来，作为重要的化学加固材料之一的聚氨酯注浆材料发展也十分迅速。并且人们将目光投向了TPU储水袋、TPU军用储油袋、TPU涉水类产品等。
将TPU作为军用储油袋是未来替代硬质油罐的理想选择。软体油袋与金属油罐相比，具有重量轻、体积小、不锈蚀、装卸运输和展开撤收方便等优点，被美军广泛应用于战场储存散装油料。特殊情况下，也可以将软体油罐置于汽车、舰船和飞机上作为运油容器，有的软体油罐还可用于空运、空投、直升机吊运、水上拖运以及水下储存油料。在成品油存储、管道抢修等众多领域中可替代传统的铁制油罐或油箱，成为一种储存和运输液体的新途径。与其它高分子材料一样，聚氨酯材料本身具有很高的表面电阻，在使用过程中容易产生静电荷积累，是造成火灾、爆炸等安全事故的重要隐患。
发明内容
本发明的目的在于针对现有技术中的不足与缺陷，提供一种军用储油袋TPU复合材料及其制备方法。经本发明方法制备的复合材料具有优异的力学与抗静电性能，阻燃性能及抗老抗黄变性能，安全环保，且热稳定性能得到了进一步提高，尤其适用于制备储水储油袋薄膜材料，具有广泛的社会经济效益以及战略价值。
为实现上述目的，本发明采用如下技术方案：
一种军用储油袋TPU复合材料：所述的TPU储油袋按重量份计，由以下成分组成：聚氨酯弹性体(TPU)100份、尼龙6(PA6)10-40份、EVA-g-MAH 5-25份、抗静电剂5-10份、改性氢氧化镁5-15份、抗氧剂0.1-0.5份、组合抗老抗黄剂1-2.5份；
所述的组合抗老抗黄剂由抗氧剂1010、紫外线吸收剂UV-232和受阻胺光稳定剂UV-622组成，其质量配比为：2:3:3。
所述的抗氧剂为抗氧剂168。
所述的抗静电剂为ATO粉，其中SnO2、Sb2O3的质量比为90:10。
所述的改性氢氧化镁的制备方法为：将氢氧化镁颗粒、3-甲基丙烯酰氧丙基三甲氧基硅烷、环己烷和正丙胺加入至三口烧瓶中，室温下搅拌30min，然后升温至60℃搅拌30min；反应结束后将悬浮液置于旋转蒸发仪中，于60℃真空状态下旋转蒸发10min，随后升温至95℃真空状态下旋转蒸发40min；最后将改性后的氢氧化镁置于80℃真空干燥箱内干燥24h，研磨后制得改性氢氧化镁颗粒。
所述的EVA-g-MAH的制备方法为：将偶氮二异丁腈与过氧化二异丙苯溶于丙酮溶液，加入乙烯-醋酸乙烯共聚物(EVA)，经干燥后与马来酸酐(MAH)一起倒入双螺杆挤出机中，挤出造粒后，经抽滤提纯后制得EVA-g-MAH。
一种制备如上任一项所述的军用储油袋TPU复合材料的方法：将干燥好的聚氨酯弹性体、尼龙6、EVA-g-MAH、抗静电剂、改性氢氧化镁、抗氧剂和组合抗老抗黄剂经混合均匀后，倒入双螺杆挤出机中挤出造粒，经烘干后由压延机压延成型制得军用储油袋TPU复合材料。
所述的军用储油袋TPU复合材料的制备方法：双螺杆挤出机在挤出造粒过程中，料筒熔融段温度控制在225℃-230℃；挤出机螺杆转速为300r/min。
本发明的有益效果在于：
(1)自制相容剂EVA-g-MAH的存在能明显降低TPU/PA6共混合金中TPU和PA6两相间的界面张力，改善了体系的相容性；
(2)本发明所制备的军用储油袋TPU复合材料膜可以大幅提高TPU材料的力学性能，同时ATO粉的存在使得复合材料的体积电阻率体积电阻急剧下降近7个数量级，达到抗静电效果，其极限氧指数(LOI)从19.5提升至27.8，经紫外光照射8小时后黄变等级达到4.1级；
(3)本发明通过加入相容剂使得TPU与PA6共混制取综合性能优良的合金来达到降低单纯使用TPU材料的成本，同时所制备的军用储油袋TPU复合材料拥有良好的抗静电性能、阻燃性能，同时通过组合抗老抗黄剂的协同作用，改善TPU易老化易黄变的缺陷；
(4)本发明制备的TPU复合材料薄膜安全环保，尤其适用于制备储水、储油袋用薄膜材料；同时，本发明适应当今市场的需求，制备方法科学合理、工序简单、操作性强，极大地提高了TPU产品的附加值，并扩展了其的应用范围，具有广泛的市场前景和显著的社会效益。
具体实施方式
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
实施例1
1)按以下配方比例及各组分要求，通过挤出造粒工艺制备得到TPU合金复合材料颗粒。
TPU树脂：100份；
PA6树脂：20份；
EVA-g-MAH：5份；
ATO粉：5份；
组合抗老抗黄剂：1份；
抗氧剂168：0.2份；
改性氢氧化镁：5份；
2)将干燥好的聚氨酯弹性体、尼龙6、EVA-g-MAH、抗静电剂、改性氢氧化镁、抗氧剂和组合抗老抗黄剂经混合均匀后，倒入双螺杆挤出机中挤出造粒，经烘干后由压延机压延成型制得军用储油袋TPU复合材料；双螺杆挤出机在挤出造粒过程中，料筒熔融段温度控制在225℃；挤出机螺杆转速为300r/min。
性能测试结果见表1。
实施例2
1)按以下配方比例及各组分要求，通过挤出造粒工艺制备得到TPU合金复合材料颗粒。
TPU树脂：100份；
PA6树脂：30份；
EVA-g-MAH：15份；
ATO粉：7份；
组合抗老抗黄剂：1.7份；
抗氧剂168：0.2份；
改性氢氧化镁：10份；
2)将干燥好的聚氨酯弹性体、尼龙6、EVA-g-MAH、抗静电剂、改性氢氧化镁、抗氧剂和组合抗老抗黄剂经混合均匀后，倒入双螺杆挤出机中挤出造粒，经烘干后由压延机压延成型制得军用储油袋TPU复合材料；双螺杆挤出机在挤出造粒过程中，料筒熔融段温度控制在230℃；挤出机螺杆转速为300r/min。
性能测试结果见表1。
实施例3
1)按以下配方比例及各组分要求，通过挤出造粒工艺制备得到TPU合金复合材料颗粒。
TPU树脂：100份；
PA6树脂：50份；
EVA-g-MAH：25份；
ATO粉：10份；
组合抗老抗黄剂：2.5份；
抗氧剂168：0.2份；
改性氢氧化镁：15份；
2)将干燥好的聚氨酯弹性体、尼龙6、EVA-g-MAH、抗静电剂、改性氢氧化镁、抗氧剂和组合抗老抗黄剂经混合均匀后，倒入双螺杆挤出机中挤出造粒，经烘干后由压延机压延成型制得军用储油袋TPU复合材料；双螺杆挤出机在挤出造粒过程中，料筒熔融段温度控制在227℃；挤出机螺杆转速为300r/min。
性能测试结果见表1。
表1本发明储油囊TPU复合材料产品与传统产品的性能对比
  传统产品 实施例1 实施例2 实施例3
拉伸强度MPa 28.3 44.65 52.74 49.28
弯曲强度MPa 28.02 25.75 24.93 21.05
缺口冲击强度KJ/m2 23.08 107.38 111.65 119.96
断裂伸长率％ 364.52 303.13 317.39 332.65
体积电阻率Ω·cm ＞1012 8.9×108 5.6×107 2.3×108
极限氧指数 19.5 25.3 27.8 27.6
黄变等级 2.0 3.5 3.8 4.1
本发明所提供的复合材料薄膜适用于制备TPU医疗床垫、TPU沼气储存袋、TPU涉水类产品、TPU储水储油袋等对材料的阻隔及抗静电性能有较高要求的领域。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。

Claims (7)

  1. 一种军用储油袋TPU复合材料，其特征在于：所述的TPU储油袋按重量份计，由以下成分组成：聚氨酯弹性体100份、尼龙6 10-40份、EVA-g-MAH 5-25份、抗静电剂5-10份、改性氢氧化镁5-15份、抗氧剂0.1-0.5份、组合抗老抗黄剂1-2.5份；所述的组合抗老抗黄剂由抗氧剂1010、紫外线吸收剂UV-232和受阻胺光稳定剂UV-622组成，其质量配比为：2:3:3。
  2. 根据权利要求1所述的军用储油袋TPU复合材料，其特征在于：所述的抗氧剂为抗氧剂168。
  3. 根据权利要求1所述的军用储油袋TPU复合材料，其特征在于：所述的抗静电剂为ATO粉，其中SnO2、Sb2O3的质量比为90:10。
  4. 根据权利要求1所述的军用储油袋TPU复合材料，其特征在于：所述的改性氢氧化镁的制备方法为：将氢氧化镁颗粒、3-甲基丙烯酰氧丙基三甲氧基硅烷、环己烷和正丙胺加入至三口烧瓶中，室温下搅拌30min，然后升温至60℃搅拌30min；反应结束后将悬浮液置于旋转蒸发仪中，于60℃真空状态下旋转蒸发10min，随后升温至95℃真空状态下旋转蒸发40min；最后将改性后的氢氧化镁置于80℃真空干燥箱内干燥24h，研磨后制得改性氢氧化镁颗粒。
  5. 根据权利要求1所述的军用储油袋TPU复合材料，其特征在于：所述的EVA-g-MAH的制备方法为：将偶氮二异丁腈与过氧化二异丙苯溶于丙酮溶液，加入乙烯-醋酸乙烯共聚物，经干燥后与马来酸酐一起倒入双螺杆挤出机中，挤出造粒后，经抽滤提纯后制得EVA-g-MAH。
  6. 一种制备如权利要求1-5任一项所述的军用储油袋TPU复合材料的方法，其特征在于：将干燥好的聚氨酯弹性体、尼龙6、EVA-g-MAH、抗静电剂、改性氢氧化镁、抗氧剂和组合抗老抗黄剂经混合均匀后，倒入双螺杆挤出机中挤出造粒，经烘干后由压延机压延成型制得军用储油袋TPU复合材料。
  7. 根据权利要求6所述的军用储油袋TPU复合材料的制备方法，其特征在于：双螺杆挤出机在挤出造粒过程中，料筒熔融段温度控制在225℃-230℃；挤出机螺杆转速为300r/min。
PCT/CN2016/106176 2016-01-07 2016-11-17 一种军用储油袋tpu复合材料及其制备方法 WO2017118222A1 (zh)

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