CN114230922A - 一种种子类剥离物高性能高掺合量复合材料的制备方法 - Google Patents
一种种子类剥离物高性能高掺合量复合材料的制备方法 Download PDFInfo
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- CN114230922A CN114230922A CN202111633110.8A CN202111633110A CN114230922A CN 114230922 A CN114230922 A CN 114230922A CN 202111633110 A CN202111633110 A CN 202111633110A CN 114230922 A CN114230922 A CN 114230922A
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Abstract
本发明公开了一种种子类剥离物高性能高掺合量复合材料的制备方法，首先根据果核、种子类生物质剥离物表面形态及极性特点，预先进行深度改性处理，使该类生物质材料的表面极性从亲水性向疏水性过渡；在降低该类生物质纤维的表面极性的同时，整理其纤维形态，提高生物质纤维的平整性和柔顺性；随后将经改性处理的生物质材料加入树脂配方体系，大幅度提高和非极性热塑性树脂的相容性，同时在配方体系中加入少量生物质长纤维增强，得到的制品不仅可以大幅度提高果核、种子类生物质剥离物掺合量，同时提升了制品的机械力学性能，不仅能作为装饰材料，也可制造出受力结构注塑制品，这对拓展质地较差的生物质的应用领域具有突破性的首创意义。
Description
技术领域
本发明涉及一种种子类剥离物高性能高掺合量复合材料的制备方法。
背景技术
果核、种子属于天然或人工种植生物质品种，这是一类品种众多、数量巨大，可再生的绿色生物质资源。它们包括咖啡壳、核桃壳、稻壳、果核壳等加工剥离物。中国稻米年产量在一亿吨以上，其加工剥离物在1500万吨以上，中国核桃等坚果剥离物占比60％，其剥离物也高达数百万吨。对这一量大面广的资源如何高值化加工应用，是人类长期不断地追求。果核、种子类生物质剥离物的特点是植物纤维中纤维素与木质素包覆紧密，质地坚硬，纤维长径比低。目前，国内外对这一类生物质剥离物复合材料的加工制品参合量少、力学指标较低，限制了它们的应用范围。这一类量大面广的生物质纤维多用于燃料、制炭或化肥、农药、饲料填充材料。
天然纤维树脂复合材料即NFC，通常以热塑性树脂聚乙烯、聚丙烯、聚氯乙烯、苯乙烯 -丙烯腈树脂、聚碳酸酯、聚乳酸、ABS中的一种或多种为基础树脂，与生物质植物纤维粉体以及相容剂、润滑剂等助剂共混，经造粒、注塑成型或挤出成型得到的环保型复合材料。其虽然是一种极具发展前景的新型绿色建材，但是，它也有着明显的不足之处。果核、种子类生物质剥离物为天然极性高分子材料，他们和大多数热塑性树脂相容性差，生物质掺合量较低，复合材料的力学性能较差，大大限制了这种新型绿色建材的应用范围。当前对生物质树脂复合材料材料的改性大多集中在提高其耐侯性、阻燃性、可润滑性等，需要添加大量的功能助剂，所加入的相容剂因配方系统为简单的机械混合，难于实现基体材料的“界面复合”，对制品力学性能改善受到局限。
发明内容
本发明针对上述现有技术所存在的问题，提供了一种种子类剥离物高性能高掺合量复合材料的制备方法，利用果核、种子类生物质剥离物制备高掺合量、高性能注塑级生物质树脂复合材料，在提高复合材料力学性能的同时能够大幅度提高生物质掺合量，从而解决复合材料中生物质掺合量与力学指标呈反比例的技术难题。本发明技术理念新颖，创造性突出，对于果核、种子类生物质剥离物高值化利用，市场应用价值高。
本发明种子类剥离物高性能高掺合量复合材料的制备方法，首先根据果核、种子类生物质剥离物表面形态及极性特点，预先进行深度改性处理，使该类生物质材料的表面极性从亲水性向疏水性过渡，同时在降低该类生物质纤维的表面极性的同时，整理其纤维形态，提高生物质纤维的平整性和柔顺性。经改性处理的果核、种子类生物质剥离物进入配方体系后，可以大幅度提高了和非极性热塑性树脂处理的相容性，再在配方系统中加入少量生物质长纤维增强，得到的制品不仅可以大幅度提高果核、种子类生物质剥离物掺合量，同时提升了制品的机械力学性能，其技术水平和工艺方法为国内外首创。
进一步地，所述果核、种子类生物质剥离物和所述生物质长纤维在添加前均需要经过深度改性处理。
所述深度改性处理包括如下步骤：
步骤1：采用甲基硅酸钠作为改性剂，对果核、种子类生物质剥离物进行改性处理，同时调整物料的pH值。具体是将果核、种子类生物质剥离物粉碎至60-800目短纤维，然后投入高速搅拌釜内，加入改性剂，调整物料pH值至7-8，在100～120℃下搅拌10～30分钟；通常植物机体呈酸性，甲基硅酸钠液体碱性，利用其优良的渗透性和成膜性达到封闭包覆的主要改性目的。
步骤2：采用EVA乳胶改性步骤1处理过的物料的表面性能。具体是向步骤1的混合物料中加入EVA乳胶和烷基苯磺酸，在100～120℃下继续搅拌10～30分钟；此过程中可以少量加入表面活性剂如十二烷基苯磺酸钠，也可以不加。
步骤3：使用纤维整理剂改善物料的平整性和柔韧性。具体是向步骤2的混合物料中加入纤维整理剂，100～120℃下继续搅拌5～20分钟；物料冷却、干燥，含水率达3％以下。
生物质长纤维的改性过程同果核、种子类生物质剥离物的改性过程，区别仅在于不需要粉碎过程。
改性后的果核、种子类生物质剥离物与改性后的生物质长纤维的添加质量之和在生物质复合材料中的质量占比为20～82％。
改性过程中各组分按质量份数构成如下：
更进一步地，所述果核、种子类生物质剥离物和所述生物质长纤维在添加前需要经过三次以上的深度改性处理。
所述果核、种子类生物质剥离物先粉碎至60-800目短纤维，再进行改性处理。
改性过程中，甲基硅酸钠是以35％固含量的水溶液形式加入。
所述生物质长纤维为纤维长度5-30mm、长径比10：1-100:1的椰丝、亚麻丝类长纤维。
所述EVA乳胶为乙烯-醋酸乙烯共聚物，固含量20-30％。
甲基硅酸钠具有碱性，且渗透性强，可渗透至毛细管内部并封闭植物纤维毛细管端口，大大降低了植物纤维的表面积和亲水性能；EVA乳胶有利于改善生物质纤维的相容性、流动性及成膜性；纤维整理剂有利于改善生物质纤维的平滑线和柔韧性。对于力学性能要求较高的复合材料，在配方体系中再加入少量经预处理的生物质长纤维，这样在复合材料体系中，经预处理后长短不一植物纤维成网状形态均匀分布并与非极性聚烯烃树脂有较好的的相容性，所得制品可以大幅度提升其综合力学性能。烷基苯磺酸钠为双亲性表面活性物质，对极性和非极性高分子物质同时具有相容性，更有利于植物纤维与非极性聚烯烃树脂的复合。
本发明高掺合量、高性能生物质树脂复合材料的加工方法，是在常规配方的基础上辅以深度改性后的果核、种子类生物质剥离物和深度改性后的生物质长纤维，经混配、造粒和注塑成型，通过更换注塑模具和调整造粒料配方，得到不同使用功能的生物质树脂复合材料注塑制品，如生活用品，文化用品，包装用品及受力结构的家具、建筑装饰制品。
具体是将常规配方和改性后的物料按配比量投入高速搅拌釜内混合均匀，然后用平行双螺杆造粒机进行造粒，最后将粒料加入注塑机进料罐，在140-180℃温度下注塑成型。
本发明工艺适用于热塑性树脂体系，如热塑性聚乙烯、聚丙烯、聚酰胺、AS树脂、聚乳酸、ABS、聚酯等。
复合材料的配方并不做具体的限定和要求，举例示意如下(按质量份数)：
所述改性植物纤维和改性长纤维的改性过程如上述所述。
所述改性无机粉体选自用1-5％钛酸酯偶联剂包覆处理的轻质碳酸钙或滑石粉，细度 800-1250目。
所述相容剂选自乙烯-马来酸酐接枝共聚物(PE-g-MAH)、三元乙丙橡胶-马来酸酐接枝共聚物(EPDM-g-MAH)、乙烯-辛烯共聚物、烷基苯磺酸钠等。
所述润滑剂为乙撑基双硬脂酸酰胺(EBS)、甲基硅油、聚乙烯蜡或硬脂酸钙、锌类内外润滑剂，可改善复合材料熔体的流动性，兼润滑、光亮和脱模剂功能，兼具热稳定性能。
所述抗氧剂选自受阻酚类抗氧剂、亚磷酸酯类抗氧剂或硫代双酚类抗氧剂，如抗氧剂 1010、1076、168/626、DLTDP、DMTDP等，用于阻止或减缓复合材料的氧化和降解。
所述紫外线吸收剂选自UV531、UV9、UV326或UV1130，具有无毒、相容性好、迁移性小、易于加工等特点。
本发明可以获得高掺合量、高性能生物质树脂复合材料，从而得以实现果核、种子类生物质剥离物的高值化利用。本发明制备的生物质树脂复合材料不仅掺合量大幅度提高，同时还可以确保制品的力学性能得到相应的提升。制品不仅可以用于众多领域装饰性注塑制品，也可以部分用于受力结构的制品。例如利用本发明技术一次成型注塑的大型大班椅，可以承受10万次以上水平疲劳冲击强调实验(纯塑料合格品标准为3万次)，样品在一次展会上被人以1580元高价买走。
本发明生物质树脂复合材料不仅可以作为装饰材料，也可作为结构材料用于受力结构家具或建筑内装饰件。对拓展该类复合材料的应用领域具有突破性的首创意义。
附图说明
图1是实施例1加工获得产品的实物照片。
图2是实施例2加工获得产品的实物照片。
图3、图4、图5是实施例3加工获得产品的实物照片。
图6是实施例4加工获得产品的实物照片。
具体实施方式
(一)植物纤维的改性
1、各组分按质量份数构成为：
所述EVA乳胶为乙烯-醋酸乙烯共聚物，固含量20-30％。
所述整理剂为聚硅氧烷。
2、改性
(1)将100份果核、种子类生物质剥离物粉碎至60-800目短纤维，然后投入高速搅拌釜内，，加入0.5～5份甲基硅酸钠乳胶，调整物料pH值至7-8，在100～120℃下搅拌10～30分钟；
(2)向步骤(1)的混合物料中加入EVA乳胶和烷基苯磺酸，在100～120℃下继续搅拌10～ 30分钟；
(3)向步骤(2)的混合物料中纤维整理剂，100～120℃下继续搅拌5～20分钟；
(4)物料冷却、干燥，含水率达3％以下，包装待用；
(5)在复合材料配方体系中需要使用长纤维增强的植物纤维改性时，改性方法参见步骤(1) -(4)。
(二)复合材料的制备
1、配方
按质量份数配方构成如下：
所述改性植物纤维和改性长纤维的改性过程如上述(一)中所述。
所述热塑性树脂为热塑性聚乙烯、聚丙烯、聚酰胺、AS树脂、聚乳酸、ABS、聚酯等。
所述改性无机粉体选自用1-5％钛酸酯偶联剂包覆处理的轻质碳酸钙或滑石粉，细度 800-1250目。
所述相容剂选自乙烯-马来酸酐接枝共聚物(PE-g-MAH)、三元乙丙橡胶-马来酸酐接枝共聚物(EPDM-g-MAH)、乙烯-辛烯共聚物、烷基苯磺酸钠等。
所述润滑剂选自乙撑基双硬脂酸酰胺(EBS)、甲基硅油、聚乙烯蜡或硬脂酸钙、锌类内外润滑剂，可改善复合材料熔体的流动性，兼润滑、光亮和脱模剂功能，兼具热稳定性能。
所述抗氧剂选自受阻酚类抗氧剂、亚磷酸酯类抗氧剂或硫代双酚类抗氧剂，如抗氧剂 1010、1076、168/626、DLTDP、DMTDP等，用于阻止或减缓复合材料的氧化和降解。
所述紫外线吸收剂选自UV531、UV9、UV326或UV1130，具有无毒、相容性好、迁移性小、易于加工等特点。
2、基体材料混合、造粒
将改性植物纤维按配方要求与热塑性树脂、改性无机粉体等原料混合，在80-120℃条件下，于高速搅拌釜内搅拌混合10-40分钟，随后通过双螺杆挤出机在140-220℃下挤出造粒，冷却后待用。
3、注塑成型
将获得的粒料加入注塑机料斗，设定注塑工艺参数，在140-280℃温度下，一次(或多次) 成型得到复合材料注塑制品。改变复合材料的工艺配方和注塑机参数及模具，可以得到不同使用功能及不同形态应用制品。上述造粒料，工艺配方适当调整后，也可以作为挤出料，在挤出机内挤出成型。
(三)改性对比试验
对比试验一：
种子类剥离物(以下简称植物纤维)改性效果对比实验，方法如下：
植物纤维的改性：
1、各组分按质量份数构成为：
所述EVA乳胶为乙烯-醋酸乙烯共聚物，固含量20-30％。
所述整理剂为聚硅氧烷。
2、改性
(1)将植物纤维剥离物粉碎至60目，然后投入高速搅拌釜内，加入0～5份甲基硅酸钠乳胶，调整物料pH值至7-8，在100～120℃下搅拌10～30分钟；
(2)向步骤(1)的混合物料中加入EVA乳胶和烷基苯磺酸，在100～120℃下继续搅拌10～ 30分钟；
(3)向步骤(2)的混合物料中纤维整理剂，100～120℃下继续搅拌5～20分钟；
(4)物料冷却、干燥，含水率达3％以下，包装待用；
(5)长纤维增强的植物纤维改性时，改性方法同植物纤维改性。
复合材料的配方(按质量份数)：
所述改性植物纤维和改性长纤维的改性过程如上述所述。
所述改性无机粉体选自用1-5％钛酸酯偶联剂包覆处理的轻质碳酸钙或滑石粉，细度800目。所述相容剂选自乙烯-马来酸酐接枝共聚物(PE-g-MAH)
所述润滑剂为乙撑基双硬脂酸酰胺(EBS)、聚乙烯蜡、锌类内外润滑剂，可改善复合材料熔体的流动性，兼润滑、光亮和脱模剂功能，兼具热稳定性能。
试验方法：
1、配方料投入高速搅拌缶内高速混配10min；
2、平行双螺杆造粒机175°造粒；
3、注塑机175°注塑样条；
4、自然时效≥24H检测。
非限定实施例叙述如下：
实施例1：用于受力结构大型注塑件——大班椅
1、复合材料的配方按质量份数构成为：
2、性能测试数据
注：生物质复合材料的传统做法通常并不对生物质进行改性直接使用，表中的“传统制品”为对本制品配方中植物纤维及植物长纤维未做改性处理的对比组。
实施例2：宠物玩具——狗骨棒
1、复合材料的配方按质量份数构成为：
2、性能测试数据
注：生物质复合材料的传统做法通常并不对生物质进行改性直接使用，表中的“传统制品”为对本制品配方中植物纤维及未做改性处理的对比组。
实施例3：生活日用注塑制品
1、复合材料的配方按质量份数构成为：
2、性能测试数据
注：生物质复合材料的传统做法通常并不对生物质进行改性直接使用，表中的“传统制品”为对本制品配方中植物纤维及未做改性处理的对比组。
实施例4：大型垃圾桶
1、复合材料的配方按质量份数构成为：
2、性能测试数据
注：生物质复合材料的传统做法通常并不对生物质进行改性直接使用，表中的“传统制品”为对本制品配方中植物纤维及未做改性处理的对比组。
结果表明，传统木塑材料的力学性能和材料模量复合GB/T29418-2012标准规定。本复合材料较之传统生物质复合材料材料则有大幅度提高。因此本复合材料不仅作为装饰材料，也可以作为受力结构注塑制品。
Claims (10)
1.一种种子类剥离物高性能高掺合量复合材料的制备方法，其特征在于：
首先根据果核、种子类生物质剥离物表面形态及极性特点，预先进行深度改性处理，使该类生物质材料的表面极性从亲水性向疏水性过渡；在降低该类生物质纤维的表面极性的同时，整理其纤维形态，提高生物质纤维的平整性和柔顺性；随后将经改性处理的果核、种子类生物质剥离物加入树脂配方体系，大幅度提高和非极性热塑性树脂的相容性，同时在配方体系中加入少量生物质长纤维增强，得到的制品不仅可以大幅度提高果核、种子类生物质剥离物掺合量，同时提升了制品的机械力学性能。
2.根据权利要求1所述的制备方法，其特征在于：
在常规热塑性树脂配方体系的基础上辅以深度改性后的果核、种子类生物质剥离物和深度改性后的生物质长纤维，经混配、造粒和注塑成型，通过更换注塑模具和调整造粒料配方，得到不同使用功能的生物质树脂复合材料注塑制品。
3.根据权利要求2所述的制备方法，其特征在于：
改性后的果核、种子类生物质剥离物与改性后的生物质长纤维的添加质量之和在生物质复合材料中的质量占比为20～82％。
4.根据权利要求2所述的制备方法，其特征在于果核、种子类生物质剥离物的深度改性包括如下步骤：
步骤1：将果核、种子类生物质剥离物粉碎至60-800目短纤维，然后投入高速搅拌釜内，加入改性剂甲基硅酸钠，调整物料pH值至7-8，在100～120℃下搅拌10～30分钟；
步骤2：向步骤1的混合物料中加入EVA乳胶、烷基苯磺酸和表面活性剂，在100～120℃下继续搅拌10～30分钟；
步骤3：使用纤维整理剂改善物料的平整性和柔韧性。
5.根据权利要求4所述的制备方法，其特征在于改性过程中各组分按质量份数构成如下：
6.根据权利要求4或5所述的制备方法，其特征在于
所述果核、种子类生物质剥离物的深度改性过程重复3次以上。
7.根据权利要求2所述的制备方法，其特征在于生物质长纤维的深度改性包括如下步骤：
步骤1：将生物质长纤维投入高速搅拌釜内，加入改性剂甲基硅酸钠，调整物料pH值至7-8，在100～120℃下搅拌10～30分钟；
步骤2：向步骤1的混合物料中加入EVA乳胶、烷基苯磺酸和表面活性剂，在100～120℃下继续搅拌10～30分钟；
步骤3：使用纤维整理剂改善物料的平整性和柔韧性。
8.根据权利要求7所述的制备方法，其特征在于改性过程中各组分按质量份数构成如下：
9.根据权利要求7或8所述的制备方法，其特征在于：
所述生物质长纤维为纤维长度5-30mm、长径比10：1-100:1的椰丝、亚麻丝类长纤维。
10.根据权利要求7或8所述的制备方法，其特征在于：
所述生物质长纤维的深度改性过程重复3次以上。
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