CN109265862A - 一种木塑复合材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种木塑复合材料,以重量份数比计,由以下原料制备而成:纤维素纳米纤维0.1‑5份,植物纤维粉5‑30份,聚氯乙烯颗粒30‑90份,纳米碳酸钙25‑80份,纳米氧化锌0.5‑2份,AC发泡剂1‑5份,偶联剂0.5‑2份,润滑剂0.5‑3份。本发明的木塑复合材料中,添加了纤维素纳米纤维,纤维素纳米纤维是一种从天然植物纤维中解纤至纳米级的纤维,具有高长径比、高比表面积、低热膨胀性的性质,可以有效提高木塑复合材料的韧性和抗冲击强度。而且纤维素纳米纤维在复合材料发泡过程中,可作为发泡成核点,在发泡剂作用下有助于复合材料形成微孔气泡,减小泡孔尺寸,改善泡孔结构的均匀性,这种微孔结构可以使材料轻质化、还可吸附室内产生的有机挥发气体或者甲醛等过敏性物质。
Description
技术领域
本发明属于新型材料技术领域,具体涉及一种木塑复合材料及其制备方法。
背景技术
以木粉等植物纤维与高分子树脂(如聚乙烯、聚丙烯和聚氯乙烯等)为主 要原料制造的木塑复合材料近年来在国内外得到了迅速的发展,木塑复合材料 具有耐水、耐腐、高强度、易加工等特点,可广泛用于户外园林建筑、室内装 饰材料、家具、包装材料等领域。
以竹木植物纤维粉与聚氯乙烯(PVC)树脂、碳酸钙颗粒为主要原料,通 过高温挤压成型用于制造集成墙面材料的技术也发展较快。由于该技术产品具 有装配式的特点,施工周期短,装饰效果好,赢得了装饰市场较高的认可度。 但这种木塑集成墙板在生产过程中为了提高保温节能效果、降低材料用量,通 常形成中空的形态,这往往降低了墙面的抗冲击力学性能。
发明内容
本发明的目的是提供一种具有微孔结构,抗冲击力学性能好的木塑复合材 料及其制备方法。
本发明这种木塑复合材料,以重量份数比计,由以下原料制备而成:纤维 素纳米纤维0.1-5份,植物纤维粉5-30份,聚氯乙烯颗粒30-90份,纳米碳酸钙 25-80份,纳米氧化锌0.5-2份,AC发泡剂1-5份,偶联剂0.5-2份,润滑剂0.5-3 份。
作为优选,所述的木塑复合材料,以重量份数比计,由以下原料制备而成: 纤维素纳米纤维1-3份,植物纤维粉10-15份,聚氯乙烯颗粒50-60份,纳米碳 酸钙30-50份,纳米氧化锌1-2份,AC发泡剂2-5份,偶联剂1-2份,润滑剂 1-2份。
所述的纤维素纳米纤维的直径为1-10nm,长径比大于100。
植物纤维粉为100-300目的杨木粉、竹粉两者任意比例的混合物。
偶联剂是由马来酸酐和甲基丙烯酸缩水甘油酯混合而成,马来酸酐和甲基 丙烯酸的质量比为(10-90):(10-90)。
所述木塑复合材料的制备方法,包括以下步骤:
(1)将竹材进行干燥,粉碎成竹粉;将竹粉在设定温度下置于苯和乙醇的 混合溶液进行抽提,得到抽提后的竹粉;接着将抽提后的竹粉用苯磺酸盐水溶 液进行处理,去除木质素,然后在碱性条件下,去除半纤维素,得到竹纤维素;
(2)将步骤(1)中的竹纤维素加入到含有2,2,6,6-四甲基哌啶氧化物、溴 化钠、次氯酸钠的水溶液中,然后进行搅拌翻反应,反应过程中,滴加氢氧化 钠溶液,维持溶液的pH为9~10,反应结束后,加入甲醇,并用高剪切均质机 进行处理,处理结束后,加入亚氯酸钠、过硫酸铵,进行加热处理,处理结束 后,进行离心分离,接着经过抽滤、烘干后得到纤维素纳米纤维;
(3)将植物纤维粉放入共混器,按照比例加入偶联剂,在设定条件下进行 改性处理,得改性植物纤维粉;然后按照比例加入聚氯乙烯颗粒、纳米碳酸钙、 AC发泡剂、纳米氧化锌、润滑剂步和骤(2)中的纤维素纳米纤维,混匀后得 到混合物;
(4)将步骤(3)中的混合物放入密炼机进行密炼,得固体混合物;接着 将固体混合物排入冷混机,进行降温,降至适宜温度后,排入成型机,通过螺 杆挤出机挤出,并通过模具定型、牵引和切割工序得到木塑复合材料。
所述步骤(1)中,粉碎后竹粉的粒度为100-300目;抽提设定温度为75-85℃, 苯和乙醇的混合比例为(1-2):1;抽提时间为2-5h;苯磺酸盐水溶液的质量分数 为20-60%;竹粉与苯磺酸盐溶液的质量体积比为1:(5-20)g/mL。
所述步骤(2)中,2,2,6,6-四甲基哌啶氧化物的浓度为0.2-0.5g/L,溴化钠 的浓度为2-3g/L;次氯酸钠的浓度为3-5g/L,竹纤维素与水溶液的质量体积比 为1:(10-20)g/mL;反应温度为65-80℃,反应时间为1.5-2.5h;竹纤维素与甲醇 质量体积比为1:(1-3)g/mL;均质处理时间为0.5-2h;竹纤维素、亚氯酸钠、过 硫酸铵的质量比为(100-80):(5-3):(3-2);加热处理温度为60-75℃,处理时间为 1-3h。
所述步骤(3)中,改性处理条件为55-75℃搅拌改性,改性处理时间为0.5-1h。
所述步骤(4)中,密炼条件为:密炼室温度为115-130℃,转速为50-96rpm, 密炼时间为15-60min;适宜温度为40-45℃。
本发明的有益效果:1)本发明的木塑复合材料中,添加了纤维素纳米纤维, 纤维素纳米纤维是一种从天然植物纤维中解纤至纳米级的纤维,具有高长径比、 高比表面积、低热膨胀性的性质,可以有效提高木塑复合材料的韧性和抗冲击 强度。本发明中的纤维素纳米纤维采用了亚氯酸钠、过硫酸铵进行羟基化处理, 改善了纤维素纳米纤维与树脂材料的界面相容性,有利于后期与聚氯乙烯树脂 的密炼成型;而且纤维素纳米纤维在复合材料发泡过程中,可作为发泡成核点, 在发泡剂作用下有助于复合材料形成更多细微的微孔气泡,减小泡孔尺寸,改 善泡孔结构的均匀性,这种微孔结构除了可以使材料轻质化、提高力学性能外, 还可吸附室内产生的有机挥发气体或者甲醛等过敏性物质,调整室内湿度。2)本发明采用的植物纤维粉经过偶联剂的改性处理,使植物纤维粉具有较强的极 性,提高了植物纤维粉与聚氯乙烯的界面相容性,提高了复合材料的内部结合 强度,有利于产品质量的提升。3)本发明的制备方法较一般的木塑复合材料制 造工艺增加密炼工序,有利于纤维素纳米纤维与聚氯乙烯、纳米碳酸钙等物料 充分融合,形成更加均匀的混合物料结构,对产生更加均匀的微孔结构有明显 的改善作用,并降低植物纤维粉在挤出成型工序中的炭化问题。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描 述的实施例仅仅是本发明一部分实施例,而不是全部实施例,基于本发明中的 实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他 实施例,都属于本发明保护的范围,下面就具体实施例对本发明进一步说明。
实施例1
1、纤维素纳米纤维的制备
以去青去黄的竹材为原料,将竹材干燥至含水率6%,再经粉碎成150-200 目的竹粉;将竹粉浸没在体积比为2:1的苯/乙醇的混合溶液中,接着在85℃的 条件下抽提5h,脱除抽提物后,得到抽提后的竹粉;将抽提后的竹粉采用化学 法在质量分数为40%的苯磺酸盐水溶液条件下去除木质素,竹粉与苯磺酸盐溶 液的质量体积比为1:15g/mL,再经分离木质素液后在碱性条件下去除半纤维素, 得到竹纤维素。
取100g竹纤维素,加入含有2,2,6,6-四甲基哌啶氧化物0.3g、溴化钠3g、 次氯酸钠6.0g的1.5L的水溶液中,接着在70℃条件下搅拌反应2h,反应过程 中通过滴加5%的氢氧化钠溶液,维持反应体系的pH值在10左右;反应结束后, 向反应体系中加入甲醇100mL,再经过高剪切均质机处理0.5h;高剪切均质机 处理结束后,加入亚氯酸钠5g、过硫酸铵3g,在60℃条件下处理2h后,对水 悬浊液进行离心处理,经过抽滤、烘干处理后得到纤维素纳米纤维,所制得的 纳米纤维的直径为1-10nm,长径比大于100。
2、木塑复合材料的制备
木塑材料各原料的质量份数配比为:纤维素纳米纤维2份,植物纤维粉20 份,聚氯乙烯颗粒41.5份,纳米碳酸钙30份,纳米氧化锌1.5份,AC发泡剂2 份,偶联剂1份,润滑剂2份。
将植物纤维粉20份(植物纤维粉为200-300目的杨木粉和200-300目竹粉 按照质量比重7:3得到的混合物)加入到共混器中,接着加入偶联剂1份(偶联 剂由马来酸酐和甲基丙烯酸缩水甘油酯,两者的质量比80:20),并于65℃条件 下搅拌0.5h,至混合均匀,得到改性植物纤维粉。
向含有改性植物纤维粉的共混器中按顺序加入聚氯乙烯颗粒41.5份、纤维 素纳米纤维2份、纳米碳酸钙30份、AC发泡剂2份、纳米氧化锌1.5份、润滑 剂2份混匀后,得到共混物。接着将共混物加入到密炼机中,在密炼室温度为 120℃,转速为80rpm,密炼时间为30min的条件下,进行密炼,得固体混合物。 然后将固体混合物排入冷混机中,当物料的温度降至45℃时将其排至挤出成型 机,挤出后,通过模具定型、牵引和切割等工序得到木塑复合材料。
实施例2
1、纤维素纳米纤维的制备
以去青去黄的竹材为原料,将竹材干燥至含水率6%,再经粉碎成150-250 目的竹粉;将竹粉浸没在体积比为1.5:1的苯/乙醇的混合溶液中,接着在85℃ 的条件下抽提3h,脱除抽提物后,得到抽提后的竹粉;将抽提后的竹粉采用化 学法在质量分数为20%的苯磺酸盐水溶液条件下去除木质素,竹粉与苯磺酸盐 溶液的质量体积比为1:5g/mL,再经分离木质素液后在碱性条件下去除半纤维 素,得到竹纤维素。
取100g竹纤维素,加入含有2,2,6,6-四甲基哌啶氧化物0.6g、溴化钠4.5g、 次氯酸钠4.5g的1.5L的水溶液中,接着在80℃条件下搅拌反应1.5h,反应过 程中通过滴加5%的氢氧化钠溶液,维持反应体系的pH值在10左右;反应结束 后,向反应体系中加入甲醇200mL,再经过高剪切均质机处理1.5h;高剪切均 质机处理结束后,加入亚氯酸钠4g、过硫酸铵2g,在70℃条件下处理3h后, 对水悬浊液进行离心处理,经过抽滤、烘干处理后得到纤维素纳米纤维,所制 得的纳米纤维的直径为1-10nm,长径比大于100。
2、木塑复合材料的制备
木塑材料各原料的质量份数配比为:纤维素纳米纤维5份,植物纤维粉10 份,聚氯乙烯颗粒60份,纳米碳酸钙25份,纳米氧化锌1份,AC发泡剂5份, 偶联剂1.5份,润滑剂1份。
将植物纤维粉10份(植物纤维粉为200-300目的杨木粉和200-300目竹粉 按照质量比重9:1得到的混合物)加入到共混器中,接着加入偶联剂1.5份(偶联 剂由马来酸酐和甲基丙烯酸缩水甘油酯,两者的质量比50:50),并于55℃条件 下搅拌1h,至混合均匀,得到改性植物纤维粉。
向含有改性植物纤维粉的共混器中按顺序加入聚氯乙烯颗粒60份、纤维素 纳米纤维5份、纳米碳酸钙25份、AC发泡剂5份、纳米氧化锌1份、润滑剂1 份混匀后,得到共混物。接着将共混物加入到密炼机中,在密炼室温度为115℃, 转速为50rpm,密炼时间为60min的条件下,进行密炼,得固体混合物。然后将 固体混合物排入冷混机中,当物料的温度降至40℃时将其排至挤出成型机,挤 出后,通过模具定型、牵引和切割等工序得到木塑复合材料。
实施例3
1、纤维素纳米纤维的制备
以去青去黄的竹材为原料,将竹材干燥至含水率6%,再经粉碎成200-300 目的竹粉;将竹粉浸没在体积比为1:1的苯/乙醇的混合溶液中,接着在75℃的 条件下抽提2h,脱除抽提物后,得到抽提后的竹粉;将抽提后的竹粉采用化学 法在质量分数为60%的苯磺酸盐水溶液条件下去除木质素,竹粉与苯磺酸盐溶 液的质量体积比为1:20g/mL,再经分离木质素液后在碱性条件下去除半纤维素, 得到竹纤维素。
取80g竹纤维素,加入含有2,2,6,6-四甲基哌啶氧化物0.75g、溴化钠3.25g、 次氯酸钠溶液7.5g的1.5L的水溶液中,接着在65℃条件下搅拌反应2.5h,反 应过程中通过滴加5%的氢氧化钠溶液,维持反应体系的pH值在10左右;反应 结束后,向反应体系中加入甲醇100mL,再经过高剪切均质机处理2h;高剪切 均质机处理结束后,加入亚氯酸钠5g、过硫酸铵3g,在75℃条件下处理1h后, 对水悬浊液进行离心处理,经过抽滤、烘干处理后得到纤维素纳米纤维,所制 得的纳米纤维的直径为1-10nm,长径比大于100。
2、木塑复合材料的制备
木塑材料各原料的质量份数配比为:纤维素纳米纤维1份,植物纤维粉15 份,聚氯乙烯颗粒50份,纳米碳酸钙40份,纳米氧化锌1.5份,AC发泡剂4 份,偶联剂1份,润滑剂1份。
将植物纤维粉15份(植物纤维粉为200-300目的杨木粉和200-300目竹粉 按照质量比重5:3得到的混合物)加入到共混器中,接着加入偶联剂1份(偶联 剂由马来酸酐和甲基丙烯酸缩水甘油酯,两者的质量比80:10),并于75℃条件 下搅拌0.5h,至混合均匀,得到改性植物纤维粉。
向含有改性植物纤维粉的共混器中按顺序加入聚氯乙烯颗粒50份、纤维素 纳米纤维1份、纳米碳酸钙40份、AC发泡剂4份、纳米氧化锌1.5份、润滑剂 1份混匀后,得到共混物。接着将共混物加入到密炼机中,在密炼室温度为 130℃,转速为95rpm,密炼时间为15min的条件下,进行密炼,得固体混合物。 然后将固体混合物排入冷混机中,当物料的温度降至40℃时将其排至挤出成型 机,挤出后,通过模具定型、牵引和切割等工序得到木塑复合材料。
Claims (10)
1.一种木塑复合材料,以重量份数比计,由以下原料制备而成:纤维素纳米纤维0.1-5份,植物纤维粉5-30份,聚氯乙烯颗粒30-90份,纳米碳酸钙25-80份,纳米氧化锌0.5-2份,AC发泡剂1-5份,偶联剂0.5-2份,润滑剂0.5-3份。
2.根据权利要求1所述的木塑复合材料,其特征在于,所述的木塑复合材料,以重量份数比计,由以下原料制备而成:纤维素纳米纤维1-3份,植物纤维粉10-15份,聚氯乙烯颗粒50-60份,纳米碳酸钙30-50份,纳米氧化锌1-2份,AC发泡剂2-5份,偶联剂1-2份,润滑剂1-2份。
3.根据权利要求1所述的木塑复合材料,其特征在于,所述的纤维素纳米纤维的直径为1-10nm,长径比大于100。
4.根据权利要求1所述的木塑复合材料,其特征在于,植物纤维粉为100-300目的杨木粉、竹粉两者任意比例的混合物。
5.根据权利要求1所述的木塑复合材料,其特征在于,偶联剂是由马来酸酐和甲基丙烯酸缩水甘油酯混合而成,马来酸酐和甲基丙烯酸的质量比为(10-90):(10-90)。
6.根据权利要求1所述的木塑复合材料的制备方法,包括以下步骤:
(1)将竹材进行干燥,粉碎成竹粉;将竹粉在设定温度下置于苯和乙醇的混合溶液进行抽提,得到抽提后的竹粉;接着将抽提后的竹粉用苯磺酸盐水溶液进行处理,去除木质素,然后在碱性条件下,去除半纤维素,得到竹纤维素;
(2)将步骤(1)中的竹纤维素加入到含有2,2,6,6-四甲基哌啶氧化物、溴化钠、次氯酸钠的水溶液中,然后进行搅拌翻反应,反应过程中,滴加氢氧化钠溶液,维持溶液的pH为9~10,反应结束后,加入甲醇,并用高剪切均质机进行处理,处理结束后,加入亚氯酸钠、过硫酸铵,进行加热处理,处理结束后,进行离心分离,接着经过抽滤、烘干后得到纤维素纳米纤维;
(3)将植物纤维粉放入共混器,按照比例加入偶联剂,在设定条件下进行改性处理,得改性植物纤维粉;然后按照比例加入聚氯乙烯颗粒、纳米碳酸钙、AC发泡剂、纳米氧化锌、润滑剂步和骤(2)中的纤维素纳米纤维,混匀后得到混合物;
(4)将步骤(3)中的混合物放入密炼机进行密炼,得固体混合物;接着将固体混合物排入冷混机,进行降温,降至适宜温度后,排入成型机,通过螺杆挤出机挤出,并通过模具定型、牵引和切割等工序得到木塑复合材料。
7.根据权利要求6所述的木塑复合材料,其特征在于,所述步骤(1)中,粉碎后竹粉的粒度为100-300目;抽提设定温度为75-85℃,苯和乙醇的混合比例为(1-2):1;抽提时间为2-5h;苯磺酸盐水溶液的质量分数为20-60%;竹粉与苯磺酸盐溶液的质量体积比为1:5-20g/mL。
8.根据权利要求6所述的木塑复合材料,其特征在于,所述步骤(2)中,2,2,6,6-四甲基哌啶氧化物的浓度为0.2-0.5g/L,溴化钠的浓度为2-3g/L;次氯酸钠的浓度为3-5g/L,竹纤维素与水溶液的质量体积比为1:(10-20)g/mL;反应温度为65-80℃,反应时间为1.5-2.5h;竹纤维素与甲醇质量体积比为1:(1-3)g/mL;均质处理时间为0.5-2h;竹纤维素、亚氯酸钠、过硫酸铵的质量比为(100-80):(5-3):(3-2);加热处理温度为60-75℃,处理时间为1-3h。
9.根据权利要求6所述的木塑复合材料,其特征在于,所述步骤(3)中,改性处理条件为55-75℃搅拌改性,改性处理时间为0.5-1h。
10.根据权利要求6所述的木塑复合材料,其特征在于,所述步骤(4)中,密炼条件为:密炼室温度115-130℃,转速为50-96rpm,密炼时间为15-60min;适宜温度为40-45℃。
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CN110041644A (zh) * | 2019-05-08 | 2019-07-23 | 上海擎木新材料科技有限公司 | 一种多尺度复合填充热可逆交联pvc材料及制备方法 |
CN110041644B (zh) * | 2019-05-08 | 2021-07-02 | 上海擎木新材料科技有限公司 | 一种多尺度复合填充热可逆交联pvc材料及制备方法 |
CN113072802A (zh) * | 2021-04-02 | 2021-07-06 | 湖南省林业科学院 | 一种高长径比竹纤维素纳米纤维增强的聚乳酸复合材料的制备方法 |
CN113072802B (zh) * | 2021-04-02 | 2024-01-09 | 湖南省林业科学院 | 一种高长径比竹纤维素纳米纤维增强的聚乳酸复合材料的制备方法 |
CN113717488A (zh) * | 2021-09-06 | 2021-11-30 | 桃江县大丰木业有限责任公司 | 一种抑烟阻燃型木质复合材料及其制备方法 |
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