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CN102093735B - Wood flour/polypropylene wood-plastic composite material using silane modified ammonium polyphosphate as fire retardant and preparation method thereof - Google Patents

Wood flour/polypropylene wood-plastic composite material using silane modified ammonium polyphosphate as fire retardant and preparation method thereof Download PDF

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CN102093735B
CN102093735B CN2011100217378A CN201110021737A CN102093735B CN 102093735 B CN102093735 B CN 102093735B CN 2011100217378 A CN2011100217378 A CN 2011100217378A CN 201110021737 A CN201110021737 A CN 201110021737A CN 102093735 B CN102093735 B CN 102093735B
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ammonium polyphosphate
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polypropylene
silane
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CN102093735A (en
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李丽萍
周林
郭垂根
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Northeast Forestry University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders

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  • Mechanical Engineering (AREA)
  • Dry Formation Of Fiberboard And The Like (AREA)
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Abstract

一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料及其制备方法,涉及一种木粉/聚丙烯木塑复合材料及其制备方法。解决现有以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的相容性差、力学性能低、阻燃性能差、耐热性能差的问题。木塑复合材料由木粉、聚丙烯、硅烷改性聚磷酸铵、m-TMI-g-PP偶联剂和抗氧剂制成,所述硅烷改性聚磷酸铵由聚磷酸铵和γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。制备方法:制备硅烷改性聚磷酸铵,然后将木粉、聚丙烯、硅烷改性聚磷酸铵、m-TMI-g-PP偶联剂和抗氧剂混合后经双螺杆挤出机挤出即可。本发明的木塑复合材料阻燃性能好、机械性能高,耐热性能好;工艺简单。A wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant and a preparation method thereof, relating to a wood powder/polypropylene wood-plastic composite material and a preparation method thereof. The invention solves the problems of poor compatibility, low mechanical properties, poor flame retardancy and poor heat resistance of the existing wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate as a flame retardant. The wood-plastic composite material is made of wood powder, polypropylene, silane-modified ammonium polyphosphate, m-TMI-g-PP coupling agent and antioxidant, and the silane-modified ammonium polyphosphate is made of ammonium polyphosphate and γ- Made from methacryloxypropyltrimethoxysilane. Preparation method: Prepare silane-modified ammonium polyphosphate, then mix wood powder, polypropylene, silane-modified ammonium polyphosphate, m-TMI-g-PP coupling agent and antioxidant, and extrude through twin-screw extruder That's it. The wood-plastic composite material of the invention has good flame-retardant performance, high mechanical performance, good heat resistance performance and simple process.

Description

一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料及其制备方法A wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant and its preparation method

技术领域 technical field

本发明涉及一种木粉/聚丙烯木塑复合材料及其制备方法,具体涉及以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料及其制备方法。The invention relates to a wood powder/polypropylene wood-plastic composite material and a preparation method thereof, in particular to a wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant and a preparation method thereof.

背景技术 Background technique

木塑复合材料是利用不同组元形态的农林废弃木材原料与塑料或回收塑料通过重组、复合等技术手段形成的一种环境友好型的新材料。从上世纪90年代后木塑复合材料发展非常迅速,其主要应用于室外装修、回廊板、楼梯、护栏以及少量民用消费品。木塑复合材料可以充分利用废旧木质原料和难以降解的废弃塑料原料,对于缓解目前木材资源匮乏和废旧塑料回收利用的问题提供了新的解决途径。木塑复合材料选择的塑料原料时必须考虑木质纤维材料200℃以上加速热解的特性,塑料材料熔点不能太高。目前最常用的塑料品种包括高密度聚乙烯(HDPE)、聚丙烯(PP)、聚苯乙烯(PS)和聚氯乙烯(PVC)。除PVC外,木质纤维材料和其他三种塑料都属于易燃材料,不经阻燃处理不能达到建筑内部装修设计防火规范要求,用于室内存在一定的火灾隐患。木塑复合材料作为一种新兴而广泛使用的材料,研究其燃烧特性,合理进行阻燃处理是扩展其使用范围,使产品多样化的重要手段之一。Wood-plastic composite material is an environmentally friendly new material formed by using different component forms of agricultural and forestry waste wood raw materials and plastic or recycled plastic through recombination and compounding. Since the 1990s, wood-plastic composite materials have developed very rapidly, and they are mainly used in outdoor decoration, corridor panels, stairs, guardrails and a small amount of civilian consumer products. Wood-plastic composite materials can make full use of waste wood materials and waste plastic materials that are difficult to degrade, and provide a new solution to alleviate the current shortage of wood resources and the recycling of waste plastics. When selecting plastic raw materials for wood-plastic composite materials, the characteristics of accelerated pyrolysis of wood fiber materials above 200°C must be considered, and the melting point of plastic materials should not be too high. The most commonly used plastic varieties include high-density polyethylene (HDPE), polypropylene (PP), polystyrene (PS) and polyvinyl chloride (PVC). Except for PVC, wood fiber materials and the other three types of plastics are flammable materials. Without flame retardant treatment, they cannot meet the requirements of the fire protection code for interior decoration design of buildings, and there are certain fire hazards when used indoors. As a new and widely used material, wood-plastic composite material is one of the important means to expand its application range and diversify its products by studying its combustion characteristics and reasonable flame-retardant treatment.

传统的卤系阻燃剂虽然阻燃效果较好,但由于其阻燃过程中释放出有毒和腐蚀性的卤化氢气体,对环境和人类的危害不容忽视,因而发展无卤阻燃技术成为阻燃研究领域的热点之一。在低烟、无卤素的磷系阻燃剂中尤其以聚磷酸铵(简称APP)的应用研究最为引人注目。因其含磷、含氮量高,磷-氮可发挥协同阻燃效应,阻燃效果优越,同时毒性低,使用安全,克服了含卤阻燃剂本身烟雾大、放出有毒的腐蚀性气体和燃烧多熔滴的缺陷,但研究表明由于APP为高极性的聚合物,在木塑复合材料中的分散性和结合性不好,所以加入APP后复合材料的力学性能下降,复合材料的拉伸强度、弯曲强度和冲击强度都明显下降。同时研究表明APP对木塑复合材料进行阻燃,效果不佳,添加量高,对木塑复合材料加工和力学性能等有一定影响。Although traditional halogen-based flame retardants have good flame-retardant effects, due to the release of toxic and corrosive hydrogen halide gas during the flame-retardant process, the harm to the environment and humans cannot be ignored. Therefore, the development of halogen-free flame-retardant technology has become a One of the hotspots in the field of fuel research. Among the low-smoke and halogen-free phosphorus flame retardants, the application research of ammonium polyphosphate (APP) is the most attractive. Because of its high phosphorus and nitrogen content, phosphorus-nitrogen can exert a synergistic flame retardant effect. However, the research shows that because APP is a highly polar polymer, its dispersion and bonding in wood-plastic composite materials are not good, so the mechanical properties of the composite material will decrease after adding APP, and the tensile strength of the composite material will decrease. Tensile strength, bending strength and impact strength are all significantly decreased. At the same time, studies have shown that the flame retardancy of APP on wood-plastic composite materials is not good, and the addition amount is high, which has a certain impact on the processing and mechanical properties of wood-plastic composite materials.

发明内容 Contents of the invention

本发明的目的是为了解决现有以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的相容性差、力学性能低、阻燃性能差、耐热性能差的问题,本发明提供了一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料及其制备方法,得到了同时具有良好的相容性、力学性能、耐热性能和阻燃性能的木塑复合材料。The purpose of the present invention is to solve the problems of poor compatibility, low mechanical properties, poor flame retardancy and poor heat resistance of existing wood powder/polypropylene wood-plastic composite materials that use ammonium polyphosphate as a flame retardant. Provided is a wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant and a preparation method thereof, which has good compatibility, mechanical properties, heat resistance and flame retardancy at the same time. wood-plastic composite materials.

本发明的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,按重量份由50~70份木粉、30~50份聚丙烯、15~30份硅烷改性聚磷酸铵(M-APP)、3~6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和0.1~1份抗氧剂制成,所述硅烷改性聚磷酸铵按重量份是由80~100份聚磷酸铵和0.5~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as flame retardant of the present invention consists of 50-70 parts of wood powder, 30-50 parts of polypropylene, 15-30 parts of silane modified Ammonium polyphosphate (M-APP), 3 to 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 0.1 to 1 parts It is made of antioxidant, and the silane-modified ammonium polyphosphate is made of 80-100 parts of ammonium polyphosphate and 0.5-2 parts of γ-methacryloxypropyl trimethoxysilane in parts by weight.

本发明的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法是通过以下步骤实现的:一、按重量份将80~100份聚磷酸铵、0.5~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中,在60℃下搅拌1h,然后抽滤,然后将滤饼置于烘箱中,在105℃条件下烘干3h,得硅烷改性聚磷酸铵(M-APP),其中聚磷酸铵重量与无水乙醇体积的比例为80~100g∶150mL;二、按重量份称取如下原料:50~70份木粉、30~50份聚丙烯、15~30份步骤一制备的硅烷改性聚磷酸铵、3~6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和0.1~1份抗氧剂;三、将步骤二称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料。The preparation method of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as flame retardant of the present invention is realized through the following steps: 1. Mix 80-100 parts of ammonium polyphosphate, 0.5- Put 2 parts of γ-methacryloxypropyltrimethoxysilane and absolute ethanol into a three-necked flask, stir at 60°C for 1 hour, then filter with suction, and then put the filter cake in an oven at 105°C Drying at lower temperature for 3 hours to obtain silane-modified ammonium polyphosphate (M-APP), wherein the ratio of the weight of ammonium polyphosphate to the volume of absolute ethanol is 80-100g: 150mL; 2. Weigh the following raw materials in parts by weight: 50-70 Parts of wood flour, 30-50 parts of polypropylene, 15-30 parts of silane-modified ammonium polyphosphate prepared in step 1, 3-6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene Coupling agent and 0.1 to 1 part of antioxidant; 3. Mix and stir the raw materials weighed in step 2 to obtain a mixture, and then input the mixture into a feeder with metering, and adjust the feeding speed to 5r min -1 , and then sent into the twin-screw extruder, set the screw temperature of each section of the twin-screw extruder from the feed port to the machine head to be 160°C, 170°C, 170°C, 180°C, 180°C, 175°C ℃, 165℃, 160℃, the screw speed is 40r·min -1 , the length-to-diameter ratio of the twin-screw extruder is 35:1, after the mixture is extruded by the twin-screw extruder, it can be cooled to obtain silane-modified polymer Ammonium phosphate as flame retardant wood flour/polypropylene wood-plastic composites.

本发明以硅烷偶联剂(γ-甲基丙烯酰氧基丙基三甲氧基硅烷,KH-570)改性聚磷酸铵(简称为M-APP)为无卤阻燃剂,大幅度改进木粉/聚丙烯复合材料的阻燃性能、物理机械性能及耐热性能,提高了硅烷改性聚磷酸铵与木粉之间的相容性,使该新材料在各项性能方面都优于现有的阻燃型木粉/聚丙烯复合材料。The present invention uses silane coupling agent (γ-methacryloxypropyltrimethoxysilane, KH-570) modified ammonium polyphosphate (abbreviated as M-APP) as a halogen-free flame retardant, greatly improving wood The flame retardancy, physical and mechanical properties and heat resistance of the powder/polypropylene composite material have improved the compatibility between the silane-modified ammonium polyphosphate and wood flour, making the new material better than the existing ones in all aspects. Some flame retardant wood flour / polypropylene composites.

本发明以KH-570改性聚磷酸铵,KH-570改善了聚磷酸铵(APP)的界面相容性和分散性,提高了APP在复合材料中的分散能力和结合能力,从而提高了复合材料的力学性能。The present invention uses KH-570 to modify ammonium polyphosphate, and KH-570 improves the interfacial compatibility and dispersibility of ammonium polyphosphate (APP), improves the dispersibility and binding ability of APP in composite materials, thereby improving the composite The mechanical properties of the material.

本发明的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料在受热过程中,硅烷改性聚磷酸铵(M-APP)释放出磷酸,HPO自由基、PO自由基、Si-O、Si-C和有机基团等,它们可以捕获木粉释放出来的自由基,使木粉加快分解成炭,使木粉分解时间提前,从而使聚丙烯变得稳定,推迟分解达到阻燃效果。同时M-APP可以促进炭层生成,阻止燃烧过程中的热传递和可燃性气体交换,可以在高温保护聚丙烯稳定,使其分解温度推迟,由此可见,加入M-APP阻燃剂使复合材料的热降解行为得到更好的改善。In the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as flame retardant of the present invention, during the heating process, silane-modified ammonium polyphosphate (M-APP) releases phosphoric acid, HPO free radicals, PO free radicals radicals, Si-O, Si-C and organic groups, etc., they can capture the free radicals released by wood powder, accelerate the decomposition of wood powder into charcoal, and advance the decomposition time of wood powder, so that polypropylene becomes stable and delays Decomposition achieves flame retardant effect. At the same time, M-APP can promote the formation of charcoal layer, prevent heat transfer and flammable gas exchange in the combustion process, and can protect the stability of polypropylene at high temperature and delay its decomposition temperature. It can be seen that adding M-APP flame retardant makes the compound The thermal degradation behavior of the material is better improved.

本发明的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料(简记为M-APP木粉/PP材料)的力学性能好,拉伸强度为24.93~28.04MPa,弯曲强度为61.98~65.68MPa,冲击强度为4.11~5.75kJ/m2;而现有以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料(简记为APP木粉/PP材料,按重量份由25份APP、60份木粉、40份PP、6份m-TMI-g-PP偶联剂和1份抗氧剂制成)的拉伸强度为21.88MPa,弯曲强度为59.87MPa,冲击强度为3.39kJ/m2;未加阻燃剂的木粉/聚丙烯木塑复合材料(简记为木粉/PP材料)的拉伸强度为23.27MPa,弯曲强度为60.29MPa,冲击强度为3.94kJ/m2。可见,本发明的M-APP木粉/PP材料的力学性能比现有APP木粉/PP材料和木粉/PP材料的力学性能好,解决了现有由于聚磷酸铵阻燃剂的加入导致木粉/PP材料的力学性能下降的问题。The wood powder/polypropylene wood-plastic composite material (abbreviated as M-APP wood powder/PP material) of the present invention using silane-modified ammonium polyphosphate as a flame retardant has good mechanical properties, and the tensile strength is 24.93-28.04MPa , the bending strength is 61.98-65.68MPa, and the impact strength is 4.11-5.75kJ/m 2 ; while the existing wood powder/polypropylene wood-plastic composite material (abbreviated as APP wood powder/PP) with ammonium polyphosphate as flame retardant Material, made by weight of 25 parts of APP, 60 parts of wood powder, 40 parts of PP, 6 parts of m-TMI-g-PP coupling agent and 1 part of antioxidant) the tensile strength is 21.88MPa, and the bending strength is 59.87MPa, and the impact strength is 3.39kJ/m 2 ; the tensile strength of wood powder/polypropylene wood-plastic composite material (referred to as wood powder/PP material) without flame retardant is 23.27MPa, and the bending strength is 60.29 MPa, the impact strength is 3.94kJ/m 2 . Visible, the mechanical property of M-APP wood powder/PP material of the present invention is better than the mechanical property of existing APP wood powder/PP material and wood powder/PP material, has solved existing due to the addition of ammonium polyphosphate flame retardant The problem of the decline in the mechanical properties of wood flour/PP materials.

本发明的M-APP木粉/PP材料的耐热性能好,起始分解时间缩短,促进了M-APP木粉/PP材料成炭。本发明的M-APP木粉/PP材料的重量损失1%时的温度(T1wt%)为102.3~108.3℃,分解最高峰温度值(Tmax1)为322.9~339.2℃,聚丙烯分解最高峰温度值(Tmax2)为499.6~519.6℃,800℃时的残炭质量为21.3%~22.7%。优于现有以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料(按重量份由25份APP、60份木粉、40份PP、6份m-TMI-g-PP偶联剂和1份抗氧剂制成)的耐热性能(T1wt%为110.7℃、Tmax1为329.3℃、Tmax2为518.0℃和800℃时残炭质量为20.5%)的耐热性能。The M-APP wood powder/PP material of the present invention has good heat resistance, shortens the initial decomposition time, and promotes the charcoal formation of the M-APP wood powder/PP material. The temperature (T 1wt% ) when the weight loss of the M-APP wood flour/PP material of the present invention is 1% is 102.3-108.3°C, the highest decomposition peak temperature value (T max1 ) is 322.9-339.2°C, and the highest decomposition peak of polypropylene The temperature value (T max2 ) is 499.6-519.6°C, and the residual carbon mass at 800°C is 21.3%-22.7%. It is better than the existing wood powder/polypropylene wood-plastic composite material with ammonium polyphosphate as flame retardant (25 parts by weight of APP, 60 parts of wood powder, 40 parts of PP, 6 parts of m-TMI-g-PP even The heat resistance performance (T 1wt% is 110.7°C, T max1 is 329.3°C, T max2 is 518.0°C and the carbon residue mass is 20.5% at 800°C) heat resistance performance.

本发明的M-APP木粉/PP材料的阻燃性能好,极限氧指数为28.3%~30.7%,点燃时间(TTI)达36~56s,热释放速率(HRR)小,为154.9~169.7kW/m2,总热释放量(THR)数值小,57.2~62.2MJ/m2。均优于现有以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料(按重量份由25份APP、60份木粉、40份PP、6份m-TMI-g-PP偶联剂和1份抗氧剂制成)的阻燃性能(极限氧指数为27.4%、TTI为28s、HRR为196.2kW/m2、THR为72MJ/m2)。The M-APP wood flour/PP material of the present invention has good flame retardancy, the limiting oxygen index is 28.3%-30.7%, the ignition time (TTI) is 36-56s, and the heat release rate (HRR) is small, 154.9-169.7kW /m 2 , the total heat release (THR) value is small, 57.2-62.2MJ/m 2 . All are better than the existing wood powder/polypropylene wood-plastic composite material (by weight of 25 parts of APP, 60 parts of wood powder, 40 parts of PP, 6 parts of m-TMI-g-PP) with ammonium polyphosphate as flame retardant coupling agent and 1 part antioxidant) flame retardancy (limiting oxygen index is 27.4%, TTI is 28s, HRR is 196.2kW/m 2 , THR is 72MJ/m 2 ).

综上,本发明的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点;同时,本发明的制备方法工艺简单。In summary, the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant of the present invention has the advantages of good flame retardancy, high mechanical properties, and good heat resistance; at the same time, the preparation of the present invention The method and process are simple.

附图说明 Description of drawings

图1是具体实施方式十四、十五和十六的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线图,图中曲线1为具体实施方式十四的,曲线2为具体实施方式十五的,曲线3为具体实施方式十六的;Fig. 1 is the heat release rate (HRR)-time (s) curve figure of the wood powder/polypropylene wood-plastic composite material of embodiment 14, 15 and 16 using silane-modified ammonium polyphosphate as flame retardant , the curve 1 in the figure is the fourteenth embodiment, the curve 2 is the fifteenth embodiment, and the curve 3 is the sixteenth embodiment;

图2是具体实施方式十四、十五和十六的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线图,图中曲线1为具体实施方式十四的,曲线2为具体实施方式十五的,曲线3为具体实施方式十六的;Fig. 2 is the total heat release (THR)-time (s) curve figure of the wood flour/polypropylene wood-plastic composite material of embodiment 14, 15 and 16, and curve 1 among the figure is embodiment 14 The curve 2 is the fifteenth embodiment, and the curve 3 is the sixteenth embodiment;

图3是具体实施方式十四、十五和十六的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线图,图中曲线1为具体实施方式十四的,曲线2为具体实施方式十五的,曲线3为具体实施方式十六的;Fig. 3 is the total smoke emission (TSP)-time (s) curve figure of the wood flour/polypropylene wood-plastic composite material of embodiment 14, 15 and 16, and curve 1 among the figure is embodiment 14 The curve 2 is the fifteenth embodiment, and the curve 3 is the sixteenth embodiment;

图4是具体实施方式十六、十七和十八的木粉/聚丙烯木塑复合材料的热重曲线图,图中曲线1为具体实施方式十六的,曲线2为具体实施方式十七的,曲线3为具体实施方式十八的;Fig. 4 is the thermogravimetric curve diagram of the wood flour/polypropylene wood-plastic composite material of embodiment 16, 17 and 18, curve 1 among the figure is embodiment 16, and curve 2 is embodiment 17 , curve 3 is the eighteenth of the specific embodiment;

图5是具体实施方式十六、十七和十八的木粉/聚丙烯木塑复合材料的微商热重曲线图,图中曲线1为具体实施方式十六的,曲线2为具体实施方式十七的,曲线3为具体实施方式十八的;Fig. 5 is the derivative thermogravimetric curve of wood powder/polypropylene wood-plastic composite material of embodiment 16, 17 and 18, curve 1 among the figure is embodiment 16, and curve 2 is embodiment Seventeen, the curve 3 is the eighteenth specific embodiment;

图6是具体实施方式十六、十七和十八的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线图,图中曲线1为具体实施方式十七的,曲线2为具体实施方式十八的,曲线3为具体实施方式十六的;Fig. 6 is the heat release rate (HRR)-time (s) curve figure of the wood flour/polypropylene wood-plastic composite material of embodiment 16, 17 and 18, and curve 1 among the figure is embodiment 17 , curve 2 is the eighteenth embodiment, and curve 3 is the sixteenth embodiment;

图7是具体实施方式十六、十七和十八的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线图,图中曲线1为具体实施方式十七的,曲线2为具体实施方式十八的,曲线3为具体实施方式十六的;Fig. 7 is the total heat release (THR)-time (s) curve figure of the wood powder/polypropylene wood-plastic composite material of embodiment 16, 17 and 18, and curve 1 among the figure is embodiment 17 The curve 2 is the eighteenth embodiment, and the curve 3 is the sixteenth embodiment;

图8是具体实施方式十六、十七和十八的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线图,图中曲线1为具体实施方式十七的,曲线2为具体实施方式十八的,曲线3为具体实施方式十六的;Fig. 8 is the total smoke emission (TSP)-time (s) graph of the wood powder/polypropylene wood-plastic composite material of embodiment 16, 17 and 18, and curve 1 among the figure is embodiment 17 The curve 2 is the eighteenth embodiment, and the curve 3 is the sixteenth embodiment;

图9是具体实施方式十六的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料进行阻燃性能测试后的表面炭层的扫描电子显微照片;Fig. 9 is the scanning electron micrograph of the surface charcoal layer after the fire retardant performance test of wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as flame retardant in embodiment sixteen;

图10是具体实施方式十七的的以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料进行阻燃性能测试后的表面炭层的扫描电子显微照片。Fig. 10 is a scanning electron micrograph of the surface charcoal layer of the wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate as a flame retardant according to the seventeenth embodiment after the flame retardant performance test.

具体实施方式 Detailed ways

本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意组合。The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.

具体实施方式一:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其按重量份由50~70份木粉、30~50份聚丙烯、15~30份硅烷改性聚磷酸铵(M-APP)、3~6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和0.1~1份抗氧剂制成,所述硅烷改性聚磷酸铵按重量份是由80~100份聚磷酸铵和0.5~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。Specific embodiment one: this embodiment is the wood powder/polypropylene wood-plastic composite material that uses silane-modified ammonium polyphosphate as a flame retardant, which consists of 50-70 parts of wood powder, 30-50 parts of polypropylene, 15-30 parts of silane-modified ammonium polyphosphate (M-APP), 3-6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) The silane-modified ammonium polyphosphate is made of 80-100 parts of ammonium polyphosphate and 0.5-2 parts of γ-methacryloxypropyl trimethoxy made from silane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的力学性能好,拉伸强度为24.93~28.04MPa,弯曲强度为61.98~65.68MPa,冲击强度为4.11~5.75kJ/m2;耐热性能好,重量损失1%时的温度(T1wt%)为102.3~108.3℃,分解最高峰温度值(Tmax1)为322.9~339.2℃,聚丙烯分解最高峰温度值(Tmax2)为499.6~519.6℃,800℃时的残炭质量为21.3%~22.7%;阻燃性能好,极限氧指数为28.3%~30.7%,点燃时间(TTI)达36~56s,热释放速率(HRR)小,为154.9~169.7kW/m2,总热释放量(THR)数值小,57.2~62.2MJ/m2The wood powder/polypropylene wood-plastic composite material of this embodiment using silane-modified ammonium polyphosphate as a flame retardant has good mechanical properties, with a tensile strength of 24.93-28.04MPa, a bending strength of 61.98-65.68MPa, and an impact strength of 4.11~5.75kJ/m 2 ; heat resistance is good, the temperature (T 1wt% ) at 1% weight loss is 102.3~108.3℃, the highest decomposition peak temperature value (T max1 ) is 322.9~339.2℃, and the decomposition of polypropylene is the most The peak temperature value (T max2 ) is 499.6-519.6°C, and the carbon residue mass at 800°C is 21.3%-22.7%; the flame retardancy is good, the limiting oxygen index is 28.3%-30.7%, and the ignition time (TTI) is 36-36% At 56s, the heat release rate (HRR) is small, ranging from 154.9 to 169.7kW/m 2 , and the total heat release (THR) is small, ranging from 57.2 to 62.2MJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance.

具体实施方式二:本实施方式与具体实施方式一不同的是按重量份由60份木粉、40份聚丙烯、20份硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂制成。其它参数与具体实施方式一相同。Specific embodiment two: the difference between this embodiment and specific embodiment one is by weight by 60 parts of wood flour, 40 parts of polypropylene, 20 parts of silane modified ammonium polyphosphate, 6 parts of m-isopropenyl-α, α - Made of dimethyl benzyl isocyanate grafted polypropylene coupling agent and 1 part antioxidant. Other parameters are the same as in the first embodiment.

具体实施方式三:本实施方式与具体实施方式一不同的是按重量份由60份木粉、40份聚丙烯、25份硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂制成。其它参数与具体实施方式一相同。Specific embodiment three: the difference between this embodiment and specific embodiment one is that by weight, 60 parts of wood flour, 40 parts of polypropylene, 25 parts of silane modified ammonium polyphosphate, 6 parts of m-isopropenyl-α, α - Made of dimethyl benzyl isocyanate grafted polypropylene coupling agent and 1 part antioxidant. Other parameters are the same as in the first embodiment.

具体实施方式四:本实施方式与具体实施方式一、二或三不同的是所述硅烷改性聚磷酸铵按重量份是由90~100份聚磷酸铵和1~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。其它参数与具体实施方式一、二或三相同。Embodiment 4: The difference between this embodiment and Embodiment 1, 2 or 3 is that the silane-modified ammonium polyphosphate is composed of 90 to 100 parts of ammonium polyphosphate and 1 to 2 parts of γ-methylacrylic acid in parts by weight. Acyloxypropyltrimethoxysilane. Other parameters are the same as those in Embodiment 1, 2 or 3.

具体实施方式五:本实施方式与具体实施方式一、二或三不同的是所述硅烷改性聚磷酸铵按重量份是由100份聚磷酸铵和1.5份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。其它参数与具体实施方式一、二或三相同。Embodiment 5: The difference between this embodiment and Embodiment 1, 2 or 3 is that the silane-modified ammonium polyphosphate is composed of 100 parts of ammonium polyphosphate and 1.5 parts of γ-methacryloxypropane in parts by weight. made from trimethoxysilane. Other parameters are the same as those in Embodiment 1, 2 or 3.

具体实施方式六:本实施方式与具体实施方式一至五之一不同的是所述抗氧剂为抗氧剂1010、抗氧剂1076或抗氧剂168。其它步骤及参数与具体实施方式一至五之一相同。Embodiment 6: This embodiment is different from Embodiment 1 to Embodiment 5 in that the antioxidant is antioxidant 1010 , antioxidant 1076 or antioxidant 168 . Other steps and parameters are the same as one of the specific embodiments 1 to 5.

具体实施方式七:本实施方式为具体实施方式一中所述的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,其是通过以下步骤实现的:一、按重量份将80~100份聚磷酸铵、0.5~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中,在60℃下搅拌1h,然后抽滤,然后将滤饼置于烘箱中,在105℃条件下烘干3h,得硅烷改性聚磷酸铵(M-APP),其中聚磷酸铵重量与无水乙醇体积的比例为80~100g∶150mL;二、按重量份称取如下原料:50~70份木粉、30~50份聚丙烯、15~30份步骤一制备的硅烷改性聚磷酸铵、3~6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和0.1~1份抗氧剂;三、将步骤二称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料。Embodiment 7: This embodiment is the preparation method of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant described in Embodiment 1, which is realized through the following steps: 1. Put 80-100 parts of ammonium polyphosphate, 0.5-2 parts of γ-methacryloxypropyl trimethoxysilane and absolute ethanol into a three-necked bottle by weight, stir at 60°C for 1 hour, and then Suction filtration, then put the filter cake in an oven, and dry at 105°C for 3 hours to obtain silane-modified ammonium polyphosphate (M-APP), wherein the ratio of the weight of ammonium polyphosphate to the volume of absolute ethanol is 80-100g : 150mL; 2. Take the following raw materials by weight: 50-70 parts of wood flour, 30-50 parts of polypropylene, 15-30 parts of silane-modified ammonium polyphosphate prepared in step 1, 3-6 parts of m-isopropylene base-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 0.1 to 1 part of antioxidant; 3. Mix and stir the raw materials weighed in step 2 to obtain a mixture, and then input the mixture into the belt In the metered feeder, adjust the feeding speed to 5r·min -1 , and then feed it into the twin-screw extruder. Set the temperature of each section of the twin-screw extruder from the feeding port to the head of the machine. 160°C, 170°C, 170°C, 180°C, 180°C, 175°C, 165°C, 160°C, the screw speed is 40r·min -1 , the length-to-diameter ratio of the twin-screw extruder is 35:1, and the mixture is made of After being extruded by a twin-screw extruder, the wood powder/polypropylene wood-plastic composite material can be obtained by cooling with silane-modified ammonium polyphosphate as a flame retardant.

本实施方式的制备方法工艺简单。制备得到的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为24.93~28.04MPa,弯曲强度为61.98~65.68MPa,冲击强度为4.11~5.75kJ/m2;耐热性能好,重量损失1%时的温度(T1wt%)为102.3~108.3℃,分解最高峰温度值(Tmax1)为322.9~339.2℃,聚丙烯分解最高峰温度值(Tmax2)为499.6~519.6℃,800℃时的残炭质量为21.3%~22.7%;阻燃性能好,极限氧指数为28.3%~30.7%,点燃时间(TTI)达36~56s,热释放速率(HRR)小,为154.9~169.7kW/m2,总热释放量(THR)数值小,57.2~62.2MJ/m2The preparation method of this embodiment has a simple process. The prepared wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant has the advantages of good flame retardancy, high mechanical performance and good heat resistance. Good mechanical properties, tensile strength is 24.93-28.04MPa, bending strength is 61.98-65.68MPa, impact strength is 4.11-5.75kJ/m 2 ; heat resistance is good, the temperature (T 1wt% ) when the weight loss is 1% is 102.3~108.3℃, the highest decomposition peak temperature (T max1 ) is 322.9~339.2℃, the highest polypropylene decomposition peak temperature (T max2 ) is 499.6~519.6℃, and the residual charcoal mass at 800℃ is 21.3%~22.7% ;Good flame retardancy, limiting oxygen index is 28.3%~30.7%, ignition time (TTI) is 36~56s, heat release rate (HRR) is small, 154.9~169.7kW/m 2 , total heat release (THR) The value is small, 57.2~62.2MJ/m 2 .

本实施方式中步骤一和步骤二中的重量份的标准可以不一样。The standards of the parts by weight in step 1 and step 2 in this embodiment can be different.

具体实施方式八:本实施方式与具体实施方式七不同的是步骤一中按重量份将90~100份聚磷酸铵、1~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中。其它步骤及参数与具体实施方式七相同。Embodiment 8: The difference between this embodiment and Embodiment 7 is that in step 1, 90 to 100 parts of ammonium polyphosphate, 1 to 2 parts of γ-methacryloxypropyl trimethoxysilane and Anhydrous ethanol was put into a three-necked bottle. Other steps and parameters are the same as those in Embodiment 7.

具体实施方式九:本实施方式与具体实施方式七不同的是步骤一中按重量份将100份聚磷酸铵、1.5份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中。其它步骤及参数与具体实施方式七相同。Specific embodiment nine: the difference between this embodiment and specific embodiment seven is that in step 1, 100 parts of ammonium polyphosphate, 1.5 parts of γ-methacryloxypropyl trimethoxysilane and absolute ethanol are put into into the three-neck bottle. Other steps and parameters are the same as those in Embodiment 7.

具体实施方式十:本实施方式与具体实施方式七、八或九不同的是步骤二中按重量份称取如下原料:60份木粉、40份聚丙烯、20份步骤一制备的硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂。其它步骤及参数与具体实施方式七、八或九相同。Embodiment 10: The difference between this embodiment and Embodiment 7, 8 or 9 is that the following raw materials are weighed by weight in step 2: 60 parts of wood powder, 40 parts of polypropylene, 20 parts of silane modified prepared in step 1 Ammonium polyphosphate, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1 part of antioxidant. Other steps and parameters are the same as those in Embodiment 7, 8 or 9.

具体实施方式十一:本实施方式与具体实施方式七、八或九不同的是步骤二中按重量份称取如下原料:60份木粉、40份聚丙烯、25份步骤一制备的硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂。其它步骤及参数与具体实施方式七、八或九相同。Embodiment 11: The difference between this embodiment and Embodiment 7, 8 or 9 is that the following raw materials are weighed by weight in step 2: 60 parts of wood powder, 40 parts of polypropylene, 25 parts of silane modification prepared in step 1 Ammonium polyphosphate, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1 part of antioxidant. Other steps and parameters are the same as those in Embodiment 7, 8 or 9.

具体实施方式十二:本实施方式与具体实施方式七、八或九不同的是步骤二中按重量份称取如下原料:60份木粉、40份聚丙烯、15份步骤一制备的硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂。其它步骤及参数与具体实施方式七、八或九相同。Embodiment 12: The difference between this embodiment and Embodiment 7, 8 or 9 is that the following raw materials are weighed by weight in step 2: 60 parts of wood powder, 40 parts of polypropylene, 15 parts of silane modification prepared in step 1 Ammonium polyphosphate, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1 part of antioxidant. Other steps and parameters are the same as those in Embodiment 7, 8 or 9.

具体实施方式十三:本实施方式与具体实施方式七、八或九不同的是步骤二中按重量份称取如下原料:60份木粉、40份聚丙烯、30份步骤一制备的硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂。其它步骤及参数与具体实施方式七、八或九相同。Embodiment 13: The difference between this embodiment and Embodiment 7, 8 or 9 is that the following raw materials are weighed by weight in step 2: 60 parts of wood flour, 40 parts of polypropylene, 30 parts of silane modified in step 1 Ammonium polyphosphate, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1 part of antioxidant. Other steps and parameters are the same as those in Embodiment 7, 8 or 9.

具体实施方式十四:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、15g硅烷改性聚磷酸铵(M-APP)、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成,所述硅烷改性聚磷酸铵是由100g聚磷酸铵和1.5gγ-甲基丙烯酰氧基丙基三甲氧基硅烷制成的。Specific embodiment fourteen: present embodiment is the wood flour/polypropylene wood-plastic composite material that uses silane-modified ammonium polyphosphate as flame retardant, and it is made of 60g wood flour, 40g polypropylene, 15g silane-modified ammonium polyphosphate ( M-APP), 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010, the silane The modified ammonium polyphosphate is made from 100 g of ammonium polyphosphate and 1.5 g of γ-methacryloxypropyltrimethoxysilane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为26.62MPa,弯曲强度为64.25MPa,冲击强度为4.90kJ/m2;耐热性能好,重量损失1%时的温度(T1wt%)为108.3℃,分解最高峰温度值(Tmax1)为339.2℃,聚丙烯分解最高峰温度值(Tmax2)为499.6℃,800℃时的残炭质量为21.3%;阻燃性能好,极限氧指数为28.3%,点燃时间(TTI)达36s,热释放速率(HRR)小,为169.7kW/m2,总热释放量(THR)数值小,62.2MJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, tensile strength is 26.62MPa, bending strength is 64.25MPa, impact strength is 4.90kJ/m 2 ; heat resistance is good, the temperature (T 1wt% ) when the weight loss is 1% is 108.3℃, and the highest decomposition peak The temperature value (T max1 ) is 339.2°C, the highest peak temperature value (T max2 ) of polypropylene decomposition is 499.6°C, and the residual carbon mass at 800°C is 21.3%; the flame retardancy is good, the limiting oxygen index is 28.3%, and the ignition time (TTI) up to 36s, the heat release rate (HRR) is small at 169.7kW/m 2 , and the total heat release (THR) is small at 62.2MJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线如图1中曲线1所示。The heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 1 in FIG. 1 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线如图2中曲线1所示。The total heat release (THR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 1 in FIG. 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线如图3中曲线1所示。The total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 1 in FIG. 3 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,是通过以下步骤实现的:一、按重量份将100g聚磷酸铵、1.5gγ-甲基丙烯酰氧基丙基三甲氧基硅烷和150mL无水乙醇放入三口瓶中,在60℃下搅拌1h,然后抽滤,然后将滤饼置于烘箱中,在105℃条件下烘干3h,得硅烷改性聚磷酸铵(M-APP);二、按重量份称取如下原料:60g木粉、40g聚丙烯、15g步骤一制备的硅烷改性聚磷酸铵、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1g抗氧剂1010;三、将步骤二称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料。The preparation method of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is realized through the following steps: 1. Mix 100g ammonium polyphosphate, 1.5g gamma- Put methacryloxypropyltrimethoxysilane and 150mL absolute ethanol into a three-necked flask, stir at 60°C for 1 hour, then filter with suction, then put the filter cake in an oven and dry it at 105°C 3h to obtain silane-modified ammonium polyphosphate (M-APP); 2. Take the following raw materials by weight: 60g wood flour, 40g polypropylene, 15g silane-modified ammonium polyphosphate prepared in step 1, 6g m-isopropylene Base-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1g antioxidant 1010; 3. Mix and stir the raw materials weighed in step 2 to obtain a mixture, and then input the mixture into the metering In the feeder, adjust the feeding speed to 5r·min -1 , and then feed it into the twin-screw extruder, and set the screw temperature of each section of the twin-screw extruder from the feeding port to the machine head to be 160°C . After being extruded by the extruder, the wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as the flame retardant can be obtained after cooling.

具体实施方式十五:本实施方式与具体实施方式十四不同的是以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料由60g木粉、40g聚丙烯、20g硅烷改性聚磷酸铵(M-APP)、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成。其它参数与具体实施方式十四相同。Embodiment 15: This embodiment is different from Embodiment 14 in that the wood flour/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as a flame retardant consists of 60g wood flour, 40g polypropylene, and 20g silane Modified ammonium polyphosphate (M-APP), 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 production. Other parameters are the same as in the fourteenth embodiment.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为27.1MPa,弯曲强度为65.68MPa,冲击强度为5.50kJ/m2;耐热性能好,重量损失1%时的温度(T1wt%)为104.7℃,分解最高峰温度值(Tmax1)为326.7℃,聚丙烯分解最高峰温度值(Tmax2)为512.3℃,800℃时的残炭质量为22%;阻燃性能好,极限氧指数为29.5%,点燃时间(TTI)达54s,热释放速率(HRR)小,为158.7kW/m2,总热释放量(THR)数值小,58.8MJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, tensile strength is 27.1MPa, bending strength is 65.68MPa, impact strength is 5.50kJ/m 2 ; heat resistance is good, the temperature (T 1wt% ) when the weight loss is 1% is 104.7℃, and the highest decomposition peak The temperature value (T max1 ) is 326.7°C, the highest peak temperature value (T max2 ) of polypropylene decomposition is 512.3°C, and the mass of char residue at 800°C is 22%; the flame retardancy is good, the limiting oxygen index is 29.5%, and the ignition time (TTI) up to 54s, the heat release rate (HRR) is small at 158.7kW/m 2 , and the total heat release (THR) is small at 58.8MJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线如图1中曲线2所示。The heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 2 in FIG. 1 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线如图2中曲线2所示。The total heat release (THR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 2 in FIG. 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线如图3中曲线2所示。The total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 2 in FIG. 3 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法与具体实施方式十四中记载的制备方法相比,除了步骤二中称取的硅烷改性聚磷酸铵改变为20g外,其余的步骤及参数一样。The preparation method of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is compared with the preparation method described in Embodiment 14, except that the silane weighed in step 2 Except that the modified ammonium polyphosphate is changed to 20g, all the other steps and parameters are the same.

具体实施方式十六:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、25g硅烷改性聚磷酸铵(M-APP)、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成,所述硅烷改性聚磷酸铵是由100g聚磷酸铵和1.5gγ-甲基丙烯酰氧基丙基三甲氧基硅烷制成的。Specific embodiment sixteen: present embodiment is the wood flour/polypropylene wood-plastic composite material of fire retardant with silane modified ammonium polyphosphate, it is by 60g wood flour, 40g polypropylene, 25g silane modified ammonium polyphosphate ( M-APP), 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010, the silane The modified ammonium polyphosphate is made from 100 g of ammonium polyphosphate and 1.5 g of γ-methacryloxypropyltrimethoxysilane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法与具体实施方式十四中记载的制备方法相比,除了步骤二中称取的硅烷改性聚磷酸铵改变为25g外,其余的步骤及参数一样。The preparation method of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is compared with the preparation method described in Embodiment 14, except that the silane weighed in step 2 Except that the modified ammonium polyphosphate is changed to 25g, all the other steps and parameters are the same.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为28.04MPa,弯曲强度为65.53MPa,冲击强度为5.75kJ/m2;耐热性能好,重量损失1%时的温度(T1wt%)为102.3℃,分解最高峰温度值(Tmax1)为322.9℃,聚丙烯分解最高峰温度值(Tmax2)为519.6℃,800℃时的残炭质量为22.7%;阻燃性能好,极限氧指数为30.7%,点燃时间(TTI)达56s,热释放速率(HRR)小,为154.9kW/m2,总热释放量(THR)数值小,57.2MJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, tensile strength is 28.04MPa, bending strength is 65.53MPa, impact strength is 5.75kJ/m 2 ; heat resistance is good, the temperature (T 1wt% ) when the weight loss is 1% is 102.3℃, the highest decomposition peak The temperature value (T max1 ) is 322.9°C, the highest peak temperature value (T max2 ) of polypropylene decomposition is 519.6°C, and the residual carbon mass at 800°C is 22.7%; the flame retardancy is good, the limiting oxygen index is 30.7%, and the ignition time (TTI) up to 56s, the heat release rate (HRR) is small at 154.9kW/m 2 , and the total heat release (THR) is small at 57.2MJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线如图1中曲线3所示。The heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 3 in FIG. 1 .

综合图1中各曲线可见,具体实施方式十四至十六中随着M-APP用量的增加,热释放速率(HRR)明显下降,由169.7kW/m2下降至154.9kW/m2。当M-APP用量为20份时,木塑复合材料表现出良好的阻燃效果,继续提高M-APP的用量,HRR的降低幅度变小。From the curves in Fig. 1, it can be seen that in Embodiments 14 to 16, as the amount of M-APP increases, the heat release rate (HRR) decreases significantly, from 169.7kW/m 2 to 154.9kW/m 2 . When the amount of M-APP is 20 phr, the wood-plastic composite material shows a good flame retardant effect, and the reduction of HRR becomes smaller if the amount of M-APP is continued to increase.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线如图2中曲线3所示。The total heat release (THR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 3 in FIG. 2 .

综合图2中各曲线可见,具体实施方式十四至十六中随着M-APP用量的增加,总热释放量(THR)明显变小,M-APP用量为25份时,总热释放量的减小不明显了。Integrating the curves in Fig. 2, it can be seen that in the fourteenth to sixteenth specific embodiments, with the increase of the amount of M-APP, the total heat release (THR) is significantly smaller, and when the amount of M-APP is 25 parts, the total heat release The reduction is not obvious.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线如图3中曲线3所示。The total smoke emission (TSP)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 3 in FIG. 3 .

综合图3中各曲线可见,具体实施方式十四至十六中随着M-APP用量的增加,总烟释放量(TSP)明显减小,M-APP用量为25份时,总热释放量的减小不明显了。From the curves in Fig. 3, it can be seen that in the fourteenth to sixteenth specific embodiments, with the increase of the amount of M-APP, the total smoke release (TSP) obviously decreases, and when the amount of M-APP is 25 parts, the total heat release The reduction is not obvious.

同时,采用热重分析仪测试得到的本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的热重曲线(TG曲线)和微商热重曲线(DTG曲线)分别如图4中曲线1和图5中曲线1所示。Simultaneously, the thermogravimetric curve (TG curve) and the derivative thermogravimetric curve ( DTG curve) are shown in curve 1 in Fig. 4 and curve 1 in Fig. 5 respectively.

采用锥形量热仪,依据ASTM 1356-90标准进行阻燃性能测试后的本实施方式的木塑复合材料的表面炭层的扫描电子显微照片如图9所示。由图9可以看出,加入M-APP的复合材料燃烧表面炭层较膨松,炭层较厚使材料表面产生更厚的保护膜来阻止火势的蔓延,可见KH-570可以提高APP在复合材料中的分散性和结合行,促进木粉成炭,阻止热量转移到聚丙烯(PP)同时防止氧气进入材料内部使其助燃,炭层结构是阻燃能力的首要因素,再结合锥形量热仪数据分析,力学性能的提高,说明M-APP在木塑复合材料中不止提高了材料的力学性能同时提高了阻燃性能。The scanning electron micrograph of the carbon layer on the surface of the wood-plastic composite material of this embodiment after the flame retardant performance test is carried out according to the ASTM 1356-90 standard by using a cone calorimeter is shown in FIG. 9 . It can be seen from Figure 9 that the charcoal layer on the combustion surface of the composite material added with M-APP is more bulky, and the thicker charcoal layer produces a thicker protective film on the surface of the material to prevent the spread of the fire. It can be seen that KH-570 can improve APP in the composite The dispersion and combination in the material can promote the charcoal formation of wood powder, prevent heat transfer to polypropylene (PP) and prevent oxygen from entering the material to support combustion. The charcoal layer structure is the primary factor for flame retardancy, combined with the conical The thermal instrument data analysis and the improvement of mechanical properties indicate that M-APP not only improves the mechanical properties of materials in wood-plastic composites, but also improves the flame retardancy.

具体实施方式十七:本实施方式为对比实施例一:聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、25g聚磷酸铵(APP)、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成。Specific Embodiment Seventeen: This embodiment is comparative example one: ammonium polyphosphate is the wood flour/polypropylene wood-plastic composite material of flame retardant, and it is made of 60g wood flour, 40g polypropylene, 25g ammonium polyphosphate (APP) , 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010.

制备方法为:一、按重量份称取如下原料:60g木粉、40g聚丙烯、25g聚磷酸铵、6gm-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1g抗氧剂1010;二、将步骤一称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料。The preparation method is: 1. Weigh the following raw materials by weight: 60g wood flour, 40g polypropylene, 25g ammonium polyphosphate, 6gm-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1g antioxidant 1010; 2. Mix and stir the raw materials weighed in step 1 to obtain a mixture, then input the mixture into a feeder with metering, adjust the feeding speed to 5r·min -1 , and then send Into the twin-screw extruder, set the temperature of each section of the twin-screw extruder from the feeding port to the head of the machine to be 160°C, 170°C, 170°C, 180°C, 180°C, 175°C, 165°C, 160°C, the screw speed is 40r·min -1 , the length-to-diameter ratio of the twin-screw extruder is 35:1, after the mixture is extruded by the twin-screw extruder, it is cooled to obtain wood with ammonium polyphosphate as a flame retardant Powder/polypropylene wood plastic composite.

本实施方式以没有采用硅烷改性的聚磷酸铵为阻燃剂,力学性能参数为:拉伸强度为21.88MPa,弯曲强度为59.87MPa,冲击强度为3.39kJ/m2;耐热性能参数为:重量损失1%时的温度(T1wt%)为110.7℃,分解最高峰温度值(Tmax1)为329.2℃,聚丙烯分解最高峰温度值(Tmax2)为518.0℃,800℃时的残炭质量为21.5%;阻燃性能参数为:极限氧指数为27.4%,点燃时间(TTI)达28s,热释放速率(HRR)小,为196.2kW/m2,总热释放量(THR)数值小,72MJ/m2In this embodiment, ammonium polyphosphate without silane modification is used as the flame retardant, and the mechanical performance parameters are: the tensile strength is 21.88MPa, the bending strength is 59.87MPa, and the impact strength is 3.39kJ/m 2 ; the heat resistance performance parameters are : The temperature (T 1wt% ) at 1% weight loss is 110.7°C, the highest decomposition temperature (T max1 ) is 329.2°C, the highest decomposition temperature of polypropylene (T max2 ) is 518.0°C, and the residue at 800°C The carbon mass is 21.5%; the flame retardant performance parameters are: the limiting oxygen index is 27.4%, the ignition time (TTI) is 28s, the heat release rate (HRR) is small, 196.2kW/m 2 , and the total heat release (THR) value Small, 72MJ/m 2 .

采用热重分析仪测试得到的本实施方式的以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的热重曲线(TG曲线)和微商热重曲线(DTG曲线)分别如图4中曲线2和图5中曲线2所示。图5中曲线2与曲线1对应的400℃以后的曲线几乎重合。The thermogravimetric curve (TG curve) and the derivative thermogravimetric curve (DTG curve) of the wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate as a flame retardant of the present embodiment obtained by using a thermogravimetric analyzer test are respectively as follows Curve 2 in Figure 4 and Curve 2 in Figure 5. In Fig. 5, curve 2 and the curve after 400°C corresponding to curve 1 almost coincide.

本实施方式的以聚磷酸铵(APP)为阻燃剂的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线如图6中曲线1所示。The heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate (APP) as a flame retardant in this embodiment is shown in curve 1 in FIG. 6 .

本实施方式的以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线如图7中曲线1所示。The total heat release (THR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 1 in FIG. 7 .

本实施方式的以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线如图8中曲线1所示。The total smoke emission (TSP)-time (s) curve of the wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate as a flame retardant in this embodiment is shown in curve 1 in FIG. 8 .

采用锥形量热仪,依据ASTM 1356-90标准进行阻燃性能测试后的本实施方式的木塑复合材料的表面炭层的扫描电子显微照片如图10所示。由图10可见,表面炭层薄而致密。The scanning electron micrograph of the carbon layer on the surface of the wood-plastic composite material of this embodiment after the flame retardant performance test according to the ASTM 1356-90 standard is shown in FIG. 10 using a cone calorimeter. It can be seen from Figure 10 that the surface carbon layer is thin and dense.

具体实施方式十八:本实施方式为对比实施例二:未加阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、6gm-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成。Embodiment 18: This embodiment is Comparative Example 2: wood powder/polypropylene wood-plastic composite material without flame retardant, which consists of 60g wood powder, 40g polypropylene, 6gm-isopropenyl-α, α - Made of dimethyl benzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010.

制备方法为:一、按重量份称取如下原料:60g木粉、40g聚丙烯、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1g抗氧剂1010;二、将步骤一称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得木粉/聚丙烯木塑复合材料。The preparation method is: 1. Take the following raw materials by weight: 60g wood flour, 40g polypropylene, 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1g antioxidant 1010; 2. Mix and stir the raw materials weighed in step 1 to obtain a mixture, then feed the mixture into a feeder with metering, adjust the feeding speed to 5r·min -1 , and then send it into the twin-screw extruder In the extruder, set the screw temperature of each section of the twin-screw extruder from the feed port to the machine head to be 160°C, 170°C, 170°C, 180°C, 180°C, 175°C, 165°C, 160°C, and the screw The rotation speed is 40r·min -1 , the length-to-diameter ratio of the twin-screw extruder is 35:1, and the compound is extruded by the twin-screw extruder and cooled to obtain the wood powder/polypropylene wood-plastic composite material.

本实施方式没有采用阻燃剂制备得到的木粉/聚丙烯木塑复合材料,力学性能参数为:拉伸强度为23.27MPa,弯曲强度为60.29MPa,冲击强度为3.94kJ/m2;耐热性能参数为:重量损失1%时的温度(T1wt%)为118.4℃,分解最高峰温度值(Tmax1)为383.2℃,聚丙烯分解最高峰温度值(Tmax2)为444.8℃,800℃时的残炭质量为12.6%;阻燃性能参数为:极限氧指数为23.6%,点燃时间(TTI)达33s,热释放速率(HRR)大,为357.5kW/m2,总热释放量(THR)数值大,102.1MJ/m2The wood powder/polypropylene wood-plastic composite material prepared without flame retardant in this embodiment has mechanical performance parameters: tensile strength is 23.27MPa, bending strength is 60.29MPa, impact strength is 3.94kJ/m 2 ; heat resistance The performance parameters are: the temperature at 1% weight loss (T 1wt% ) is 118.4°C, the highest decomposition peak temperature (T max1 ) is 383.2°C, the highest polypropylene decomposition peak temperature (T max2 ) is 444.8°C, 800°C The mass of residual charcoal was 12.6%; the flame retardant performance parameters were: the limiting oxygen index was 23.6%, the ignition time (TTI) was 33s, the heat release rate (HRR) was 357.5kW/m 2 , the total heat release ( THR) has a large value, 102.1MJ/m 2 .

采用热重分析仪测试得到的本实施方式的未添加阻燃剂的木粉/聚丙烯木塑复合材料的热重曲线(TG曲线)和微商热重曲线(DTG曲线)分别如图4中曲线3和图5中曲线3所示。The thermogravimetric curve (TG curve) and the derivative thermogravimetric curve (DTG curve) of the wood flour/polypropylene wood-plastic composite material without adding flame retardants of the present embodiment obtained by the thermogravimetric analyzer test are shown in Fig. 4 respectively Curve 3 and curve 3 in Figure 5.

由图4中可知,TG曲线中热降解过程经历两个平台,第一个拐点是木粉开始分解,第二个拐点是聚丙烯开始分解。由图5可见,加入APP和M-APP之后木粉的最高分解温度向低温移动,而聚丙烯的最高分解温度向高温移动。分析可知,加入APP或M-APP后木塑复合材料的起始分解时间缩短,促进复合材料成炭;与加入APP相比,加入M-APP使T 1wt%由110.7减低到102.3℃,Tmax1由329.3降低到322.9℃,Tmax2由518.0提高到519.6℃,800℃时残炭由21.5提高到22.7%。It can be seen from Figure 4 that the thermal degradation process in the TG curve experiences two platforms, the first inflection point is when wood flour begins to decompose, and the second inflection point is when polypropylene begins to decompose. It can be seen from Figure 5 that after adding APP and M-APP, the maximum decomposition temperature of wood powder moves to low temperature, while the maximum decomposition temperature of polypropylene moves to high temperature. The analysis shows that the initial decomposition time of wood-plastic composites is shortened after adding APP or M-APP, which promotes the charring of composite materials; compared with adding APP, adding M-APP can reduce T 1wt% from 110.7 to 102.3 ℃, T max1 Decreased from 329.3 to 322.9°C, T max2 increased from 518.0 to 519.6°C, and carbon residue increased from 21.5 to 22.7% at 800°C.

本实施方式的未添加阻燃剂的木粉/聚丙烯木塑复合材料的热释放速率(HRR)-时间(s)曲线如图6中曲线2所示。The heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood-plastic composite material without adding a flame retardant in this embodiment is shown in curve 2 in FIG. 6 .

本实施方式的未添加阻燃剂的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线如图7中曲线2所示。The total heat release (THR)-time (s) curve of the wood flour/polypropylene wood-plastic composite material without adding a flame retardant in this embodiment is shown in curve 2 in FIG. 7 .

本实施方式的未添加阻燃剂的木粉/聚丙烯木塑复合材料的总烟释放量(TSP)-时间(s)曲线如图8中曲线2所示。The total smoke delivery (TSP)-time (s) curve of the wood powder/polypropylene wood-plastic composite material without adding a flame retardant in this embodiment is shown in curve 2 in FIG. 8 .

为了方便对比,将具体实施方式十六的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的总热释放量(THR)-时间(s)曲线、总热释放量(THR)-时间(s)曲线和总烟释放量(TSP)-时间(s)曲线分别相应地记入图6、图7和图8中,记为曲线3。For convenience of comparison, the total heat release (THR)-time (s) curve, total heat release The amount (THR)-time (s) curve and the total smoke delivery (TSP)-time (s) curve are correspondingly recorded in Fig. 6, Fig. 7 and Fig. 8 respectively, and are marked as curve 3.

综合分析对比具体实施方式十六、十七和十八可得,具体实施方式十七的以聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的力学性能比具体实施方式十八的木粉/聚丙烯木塑复合材料的力学性能差,说明高极性聚合物聚磷酸铵的加入,其在木塑复合材料中的分散性和结合性不好,所以加入APP后木粉/聚丙烯木塑复合材料的反而力学性能下降。采用γ-甲基丙烯酰氧基丙基三甲氧基硅烷改性后的聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的力学性能比具体实施方式十八的木粉/聚丙烯木塑复合材料的力学性能提高了,说明以经硅烷改性后的聚磷酸铵在木粉/聚丙烯木塑复合材料中分散性和结合性变好,相容性变好,使得木粉/聚丙烯木塑复合材料的力学性能大大提高。Comprehensive analysis and comparison of specific embodiments 16, 17 and 18 can be obtained, and the mechanical properties of the wood powder/polypropylene wood-plastic composite material using ammonium polyphosphate as a flame retardant in the 17th embodiment are compared with the 18th embodiment The mechanical properties of wood powder/polypropylene wood-plastic composite materials are poor, indicating that the addition of highly polar polymer ammonium polyphosphate has poor dispersion and bonding in wood-plastic composite materials, so after adding APP, wood powder/polypropylene On the contrary, the mechanical properties of polypropylene wood-plastic composites decrease. Using ammonium polyphosphate modified by γ-methacryloxypropyl trimethoxysilane as the flame retardant wood flour/polypropylene wood-plastic composite material than the wood flour/polypropylene wood-plastic composite material of specific embodiment eighteen The mechanical properties of propylene wood-plastic composites have been improved, indicating that the dispersibility and bonding of ammonium polyphosphate modified by silane in wood flour/polypropylene wood-plastic composites have become better, and the compatibility has become better, making wood flour / The mechanical properties of polypropylene wood-plastic composites are greatly improved.

同时具体实施方式十六的木塑复合材料的耐热性能和阻燃性能均比具体实施方式十七的木塑复合材料的耐热性能和阻燃性能提高,变好。At the same time, the heat resistance and flame retardancy of the wood-plastic composite material in Embodiment 16 are both improved and better than those of the wood-plastic composite material in Embodiment 17.

具体实施方式十九:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、25g硅烷改性聚磷酸铵(M-APP)、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成,所述硅烷改性聚磷酸铵是由100g聚磷酸铵和0.5gγ-甲基丙烯酰氧基丙基三甲氧基硅烷制成的。Specific embodiment nineteen: present embodiment is the wood flour/polypropylene wood-plastic composite material that uses silane-modified ammonium polyphosphate as flame retardant, and it is made of 60g wood flour, 40g polypropylene, 25g silane-modified ammonium polyphosphate ( M-APP), 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010, the silane The modified ammonium polyphosphate is made from 100g of ammonium polyphosphate and 0.5g of γ-methacryloxypropyltrimethoxysilane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为24.93MPa,弯曲强度为61.98MPa,冲击强度为4.33kJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, the tensile strength is 24.93MPa, the bending strength is 61.98MPa, and the impact strength is 4.33kJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,是通过以下步骤实现的:一、按重量份将100g聚磷酸铵、0.5gγ-甲基丙烯酰氧基丙基三甲氧基硅烷和150mL无水乙醇放入三口瓶中,在60℃下搅拌1h,然后抽滤,然后将滤饼置于烘箱中,在105℃条件下烘干3h,得硅烷改性聚磷酸铵(M-APP);二、按重量份称取如下原料:60g木粉、40g聚丙烯、25g步骤一制备的硅烷改性聚磷酸铵、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1g抗氧剂1010;三、将步骤二称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料。The preparation method of the wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as flame retardant in this embodiment is realized through the following steps: 1. Mix 100g ammonium polyphosphate, 0.5g gamma- Put methacryloxypropyltrimethoxysilane and 150mL absolute ethanol into a three-necked flask, stir at 60°C for 1 hour, then filter with suction, then put the filter cake in an oven and dry it at 105°C 3h to obtain silane-modified ammonium polyphosphate (M-APP); 2. Take the following raw materials in parts by weight: 60g wood flour, 40g polypropylene, 25g silane-modified ammonium polyphosphate prepared in step 1, 6g m-isopropylene Base-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1g antioxidant 1010; 3. Mix and stir the raw materials weighed in step 2 to obtain a mixture, and then input the mixture into the metering In the feeder, adjust the feeding speed to 5r·min -1 , and then feed it into the twin-screw extruder, and set the screw temperature of each section of the twin-screw extruder from the feeding port to the machine head to be 160°C . After being extruded by the extruder, the wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as the flame retardant can be obtained after cooling.

具体实施方式二十:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、25g硅烷改性聚磷酸铵(M-APP)、6gm-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成,所述硅烷改性聚磷酸铵是由100g聚磷酸铵和1.0gγ-甲基丙烯酰氧基丙基三甲氧基硅烷制成的。Specific Embodiment Twenty: This embodiment is a wood flour/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant, which consists of 60g wood flour, 40g polypropylene, and 25g silane-modified ammonium polyphosphate ( M-APP), 6gm-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010, the silane modified The permanent ammonium polyphosphate is made from 100g of ammonium polyphosphate and 1.0g of γ-methacryloxypropyltrimethoxysilane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为25.35MPa,弯曲强度为63.03MPa,冲击强度为4.45kJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, the tensile strength is 25.35MPa, the bending strength is 63.03MPa, and the impact strength is 4.45kJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法与具体实施方式十九中记载的制备方法相比,除步骤一中γ-甲基丙烯酰氧基丙基三甲氧基硅烷的用量不同外,其余步骤及参数相同。Compared with the preparation method described in the nineteenth specific embodiment, the preparation method of the wood flour/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment, except for the γ-methyl Except the amount of acryloyloxypropyl trimethoxysilane is different, the other steps and parameters are the same.

具体实施方式二十一:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、25g硅烷改性聚磷酸铵(M-APP)、6gm-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成,所述硅烷改性聚磷酸铵是由100g聚磷酸铵和2.0gγ-甲基丙烯酰氧基丙基三甲氧基硅烷制成的。Specific Embodiment Twenty-one: This embodiment is a wood flour/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant, which consists of 60g wood flour, 40g polypropylene, and 25g silane-modified ammonium polyphosphate (M-APP), 6gm-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010, the silane The modified ammonium polyphosphate is made from 100 g of ammonium polyphosphate and 2.0 g of γ-methacryloxypropyltrimethoxysilane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为25.20MPa,弯曲强度为62.02MPa,冲击强度为4.11kJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, the tensile strength is 25.20MPa, the bending strength is 62.02MPa, and the impact strength is 4.11kJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法与具体实施方式十九中记载的制备方法相比,除步骤一中γ-甲基丙烯酰氧基丙基三甲氧基硅烷的用量不同外,其余步骤及参数相同。Compared with the preparation method described in the nineteenth specific embodiment, the preparation method of the wood flour/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment, except for the γ-methyl Except the amount of acryloyloxypropyl trimethoxysilane is different, the other steps and parameters are the same.

具体实施方式二十二:本实施方式为以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其由60g木粉、40g聚丙烯、30g硅烷改性聚磷酸铵(M-APP)、6g m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯(m-TMI-g-PP)偶联剂和1g抗氧剂1010制成,所述硅烷改性聚磷酸铵是由100g聚磷酸铵和1.5gγ-甲基丙烯酰氧基丙基三甲氧基硅烷制成的。Specific Embodiment Twenty-two: This embodiment is a wood flour/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as a flame retardant, which consists of 60g wood flour, 40g polypropylene, and 30g silane-modified ammonium polyphosphate (M-APP), 6g m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, the described The silane-modified ammonium polyphosphate is made from 100 g of ammonium polyphosphate and 1.5 g of γ-methacryloxypropyltrimethoxysilane.

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料具有阻燃性能好、机械性能高,耐热性能好的优点。力学性能好,拉伸强度为26.31MPa,弯曲强度为62.46MPa,冲击强度为4.88kJ/m2The wood powder/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment has the advantages of good flame retardancy, high mechanical performance, and good heat resistance. Good mechanical properties, the tensile strength is 26.31MPa, the bending strength is 62.46MPa, and the impact strength is 4.88kJ/m 2 .

本实施方式的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法与具体实施方式十四中记载的制备方法相比,除了步骤二中称取的硅烷改性聚磷酸铵改变为20g外,其余的步骤及参数一样。The preparation method of the wood flour/polypropylene wood-plastic composite material using silane-modified ammonium polyphosphate as a flame retardant in this embodiment is compared with the preparation method described in Embodiment 14, except that the silane weighed in step 2 Except that the modified ammonium polyphosphate is changed to 20g, all the other steps and parameters are the same.

其中,本发明中涉及到的木塑复合材料的力学性能的数据均是通过如下测试方法得到的:使用万能力学测试机测定木塑复合材料的拉伸强度和弯曲强度,使用悬臂式冲击测试机测定复合材料的冲击强度。每种样品平衡测试5次取平均值,拉伸强度测试依据ASTMD638标准,拉伸速度为5mm/min;弯曲强度测试依据ASTM D790标准,测试速度为2mm/min,跨度为64mm;冲击强度测试依据ASTM D256标准。Among them, the data of the mechanical properties of the wood-plastic composite materials involved in the present invention are all obtained by the following test methods: use a universal mechanical testing machine to measure the tensile strength and bending strength of the wood-plastic composite materials, use a cantilever impact testing machine Determination of impact strength of composite materials. The average value of each sample balance test is 5 times. The tensile strength test is based on the ASTMD638 standard, and the tensile speed is 5mm/min; the bending strength test is based on the ASTM D790 standard, the test speed is 2mm/min, and the span is 64mm; the impact strength test is based on ASTM D256 standard.

本发明中涉及到的木塑复合材料的耐热性能的数据均是通过如下测试方法得到的:使用Perkin-Elmer Pyris 1热重分析仪器对样品进行热降解行为分析,实验在纯氮气环境下进行,以升温速率为10℃·min-1从30升到800℃,每个样品重量约为3-5mg。The heat resistance data of the wood-plastic composite materials involved in the present invention are all obtained by the following test method: use the Perkin-Elmer Pyris 1 thermogravimetric analysis instrument to analyze the thermal degradation behavior of the sample, and the experiment is carried out in a pure nitrogen environment , from 30 to 800°C at a heating rate of 10°C·min -1 , and the weight of each sample is about 3-5mg.

本发明中涉及到的木塑复合材料的阻燃性能的数据均是通过如下测试方法得到的:锥形量热仪测试依据ASTM 1356-90标准,样品规格是100×100×3mm板材,采用FTTStandard锥形量热仪进行测试,采用的热辐射流量为50kW/m2The flame retardancy data of the wood-plastic composite materials involved in the present invention are all obtained by the following test method: the cone calorimeter test is based on the ASTM 1356-90 standard, and the sample size is 100×100×3mm plate, using FTTStandard Cone calorimeter is used for testing, and the heat radiation flow rate adopted is 50kW/m 2 .

Claims (10)

1.一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其特征在于以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料按重量份由50~70份木粉、30~50份聚丙烯、15~30份硅烷改性聚磷酸铵、3~6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和0.1~1份抗氧剂制成,所述硅烷改性聚磷酸铵按重量份是由80~100份聚磷酸铵和0.5~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。1. A wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as flame retardant, characterized in that the wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as flame retardant In parts by weight, it is composed of 50-70 parts of wood flour, 30-50 parts of polypropylene, 15-30 parts of silane-modified ammonium polyphosphate, and 3-6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate. Branched polypropylene coupling agent and 0.1-1 part of antioxidant, the silane-modified ammonium polyphosphate is composed of 80-100 parts of ammonium polyphosphate and 0.5-2 parts of γ-methacryloyloxy Propyltrimethoxysilane. 2.根据权利要求1所述的一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其特征在于以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料按重量份由60份木粉、40份聚丙烯、20份硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂制成。2. A kind of wood powder/polypropylene wood-plastic composite material taking silane-modified ammonium polyphosphate as fire retardant according to claim 1, it is characterized in that the wood powder taking silane-modified ammonium polyphosphate as fire retardant / Polypropylene wood-plastic composite material is grafted by weight by 60 parts of wood flour, 40 parts of polypropylene, 20 parts of silane-modified ammonium polyphosphate, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate Made of polypropylene coupling agent and 1 part antioxidant. 3.根据权利要求1所述的一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其特征在于以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料按重量份由60份木粉、40份聚丙烯、25份硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂制成。3. A kind of wood powder/polypropylene wood-plastic composite material taking silane-modified ammonium polyphosphate as fire retardant according to claim 1, it is characterized in that the wood powder taking silane-modified ammonium polyphosphate as fire retardant / Polypropylene wood-plastic composite material is grafted by weight by 60 parts of wood flour, 40 parts of polypropylene, 25 parts of silane-modified ammonium polyphosphate, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate Made of polypropylene coupling agent and 1 part antioxidant. 4.根据权利要求1、2或3所述的一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其特征在于所述硅烷改性聚磷酸铵按重量份是由90~100份聚磷酸铵和1~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。4. according to claim 1,2 or 3, a kind of wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as flame retardant, is characterized in that described silane-modified ammonium polyphosphate is by weight One part is made of 90-100 parts of ammonium polyphosphate and 1-2 parts of γ-methacryloxypropyl trimethoxysilane. 5.根据权利要求1、2或3所述的一种以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料,其特征在于所述硅烷改性聚磷酸铵按重量份是由100份聚磷酸铵和1.5份γ-甲基丙烯酰氧基丙基三甲氧基硅烷制成。5. according to claim 1,2 or 3 described a kind of wood flour/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as flame retardant, it is characterized in that described silane-modified ammonium polyphosphate is by weight Parts are made from 100 parts ammonium polyphosphate and 1.5 parts gamma-methacryloxypropyltrimethoxysilane. 6.如权利要求1所述的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,其特征在于以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法是通过以下步骤实现的:一、按重量份将80~100份聚磷酸铵、0.5~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中,在60℃下搅拌1h,然后抽滤,然后将滤饼置于烘箱中,在105℃条件下烘干3h,得硅烷改性聚磷酸铵,其中聚磷酸铵重量与无水乙醇体积的比例为80~100g∶150mL;二、按重量份称取如下原料:50~70份木粉、30~50份聚丙烯、15~30份步骤一制备的硅烷改性聚磷酸铵、3~6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和0.1~1份抗氧剂;三、将步骤二称取的原料混合搅拌均匀得混合料,然后将混合料输入带有计量的喂料器中,调节喂料转速为5r·min-1,然后再送入双螺杆挤出机中,设置双螺杆挤出机的各段螺杆温度从加料口到机头的温度分别为160℃、170℃、170℃、180℃、180℃、175℃、165℃、160℃,螺杆转速为40r·min-1,双螺杆挤出机的长径比为35∶1,混合料由双螺杆挤出机挤出后,冷却即得以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料。6. as claimed in claim 1 with silane modified ammonium polyphosphate as the preparation method of wood powder/polypropylene wood-plastic composite material of flame retardant, it is characterized in that the wood powder with silane modified ammonium polyphosphate as flame retardant The preparation method of the powder/polypropylene wood-plastic composite material is realized through the following steps: 1. Mix 80 to 100 parts of ammonium polyphosphate, 0.5 to 2 parts of γ-methacryloxypropyltrimethoxysilane in parts by weight and absolute ethanol in a three-necked flask, stirred at 60°C for 1 hour, then suction filtered, then put the filter cake in an oven, and dried at 105°C for 3 hours to obtain silane-modified ammonium polyphosphate, of which The ratio of ammonium weight to absolute ethanol volume is 80-100g: 150mL; 2. Weigh the following raw materials by weight: 50-70 parts of wood flour, 30-50 parts of polypropylene, 15-30 parts of silane modified Ammonium polyphosphate, 3 to 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 0.1 to 1 part of antioxidant; 3. The raw materials weighed in step 2 Mix and stir evenly to obtain the compound, then input the compound into the feeder with metering, adjust the feeding speed to 5r·min -1 , and then send it into the twin-screw extruder, set each of the twin-screw extruder The temperature of the section screw from the feeding port to the machine head is 160°C, 170°C, 170°C, 180°C, 180°C, 175°C, 165°C, 160°C, the screw speed is 40r·min -1 , the twin-screw extrusion The aspect ratio of the extruder is 35:1. After the mixture is extruded by the twin-screw extruder, it is cooled to obtain the wood powder/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as the flame retardant. 7.根据权利要求6所述的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,其特征在于步骤一中按重量份将90~100份聚磷酸铵、1~2份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中。7. the preparation method of wood flour/polypropylene wood-plastic composite material with silane-modified ammonium polyphosphate as fire retardant according to claim 6, it is characterized in that in step 1, 90~100 parts of polyphosphoric acid are added by weight Ammonium, 1 to 2 parts of γ-methacryloxypropyltrimethoxysilane and absolute ethanol are put into a three-necked bottle. 8.根据权利要求6所述的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,其特征在于步骤一中按重量份将100份聚磷酸铵、1.5份γ-甲基丙烯酰氧基丙基三甲氧基硅烷和无水乙醇放入三口瓶中。8. the preparation method of the wood powder/polypropylene wood-plastic composite material taking silane-modified ammonium polyphosphate as flame retardant according to claim 6 is characterized in that in step 1, 100 parts of ammonium polyphosphate, ammonium polyphosphate, Put 1.5 parts of γ-methacryloxypropyltrimethoxysilane and absolute ethanol into a three-neck bottle. 9.根据权利要求6、7或8所述的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,其特征在于步骤二中按重量份称取如下原料:60份木粉、40份聚丙烯、20份步骤一制备的硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂。9. according to the preparation method of the wood flour/polypropylene wood-plastic composite material of fire retardant with silane modified ammonium polyphosphate according to claim 6, 7 or 8, it is characterized in that in step 2, take by weight as follows Raw materials: 60 parts of wood flour, 40 parts of polypropylene, 20 parts of silane-modified ammonium polyphosphate prepared in step 1, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1 part antioxidant. 10.根据权利要求6、7或8所述的以硅烷改性聚磷酸铵为阻燃剂的木粉/聚丙烯木塑复合材料的制备方法,其特征在于步骤二中按重量份称取如下原料:60份木粉、40份聚丙烯、25份步骤一制备的硅烷改性聚磷酸铵、6份m-异丙烯基-α,α-二甲基苄基异氰酸酯接枝聚丙烯偶联剂和1份抗氧剂。10. according to the preparation method of the wood flour/polypropylene wood-plastic composite material of fire retardant with silane-modified ammonium polyphosphate according to claim 6, 7 or 8, it is characterized in that in step 2, take by weight as follows Raw materials: 60 parts of wood flour, 40 parts of polypropylene, 25 parts of silane-modified ammonium polyphosphate prepared in step 1, 6 parts of m-isopropenyl-α, α-dimethylbenzyl isocyanate grafted polypropylene coupling agent and 1 part antioxidant.
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