CN112646112B - 生物基聚氨酯泡沫及其制备方法 - Google Patents

生物基聚氨酯泡沫及其制备方法 Download PDF

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CN112646112B
CN112646112B CN202011465445.9A CN202011465445A CN112646112B CN 112646112 B CN112646112 B CN 112646112B CN 202011465445 A CN202011465445 A CN 202011465445A CN 112646112 B CN112646112 B CN 112646112B
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杜孝林
李欣
张佳佳
林壮
王许
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Shandong Inov New Material Co Ltd
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Abstract

本发明涉及聚氨酯技术领域,具体涉及一种生物基聚氨酯泡沫及其制备方法。所述的生物基聚氨酯泡沫,由A组分和B组分按质量比1:1.0~1.5混合制成;以质量百分数计,A组分由以下原料组成:木质素30~60%,聚己内酯20~30%,聚醚多元醇10~20%,交联剂3~5%,匀泡剂A1~2%,匀泡剂B1~2%,水0.5~10%,催化剂0.3~1.5%,填料0~20%;B组分为异佛尔酮二异氰酸酯。本发明的生物基聚氨酯泡沫,具有高吸水性,高开孔率和良好的机械强度,应用于仿生土壤,插花泥等领域,具有可生物降解性,降解产物对环境及土壤不会造成污染;本发明还提供其制备方法。

Description

生物基聚氨酯泡沫及其制备方法
技术领域
本发明涉及聚氨酯技术领域,具体涉及一种生物基聚氨酯泡沫及其制备方法。
背景技术
聚氨酯泡沫塑料易成型,加工方便,原料易得,所得制品具有优异的机械性能、声学性能、电学性能和耐化性能,在国民生产建设中起到举足轻重的作用。
由于聚氨酯泡沫具有孔隙大、气泡均匀、密度低、透气、耐温、耐老化、抗水和抗溶剂侵蚀等特性,且具有吸水、保水能力,近年来,聚氨酯泡沫开始应用于插花泥领域。插花泥在花卉市场销量很大,是一种具有开发价值的新产品,能有效地延长鲜花观赏期,该产品既适用于做插花泥,也可用作花卉培养土。然而,聚氨酯泡沫作为一种热塑性塑料,大量的废旧泡沫长时间存在于自然环境中无法降解,对环境造成严重污染。
专利CN201911274384.5中公开了一种聚氨酯插花泥材料,包括质量比为1:0.9-1.1的甲组分和乙组分,甲组分由聚醚多元醇A、聚醚多元醇B、聚醚多元醇C、聚醚多元醇D、化学发泡剂、催化剂、泡沫稳定剂以及添加剂组成;乙组分为聚合二苯基甲烷二异氰酸酯;其制备的聚氨酯插花泥材料,具有密度及颜色可调节、开孔率高、吸水性好、发泡体系环保的优点。但是其生物降解性较差,环境友好性差。
专利CN201710575690.7中公开了一种高开孔率生物质基硬质聚氨酯泡沫,按组分重量份数计,由生物基多元醇混合物100份,多异氰酸酯105-160份,复合催化剂1.05-1.4份,复合发泡剂2-6.5份,匀泡剂1.5-3.0份组成;所得到的产品具有高开孔率,使用的发泡剂不含卤素,多元醇为生物质基多元醇,更环保,且辅助发泡剂为沸程型物质,使发泡过程更加温和稳定;该聚氨酯泡沫适用于制作花泥等对泡沫开孔率、吸水率要求较高的材料。但是其生物基多元醇混合物的制备方法较为复杂,且制品的密度较高,产品的成本高,生物降解性也较差。
发明内容
本发明的目的是提供一种生物基聚氨酯泡沫,具有高吸水性,高开孔率和良好的机械强度,应用于仿生土壤,插花泥等领域,具有可生物降解性,在土壤掩埋条件下通过水分和微生物的作用可进行较快速度的降解,降解产物对环境及土壤不会造成污染;本发明还提供其制备方法。
本发明所述的生物基聚氨酯泡沫,由A组分和B组分按质量比1:1.0~1.5混合制成;
以质量百分数计,A组分由以下原料组成:
Figure BDA0002833996290000021
B组分为异佛尔酮二异氰酸酯(IPDI)。
木质素的分子量为1513.58,熔点为154~162℃。
聚己内酯的羟值为200~240mgKOH/g,官能度为2,30℃黏度为250~350mpa·s,水分含量≤0.05wt%;优选为PCL205,生产厂家为湖南聚仁化工新材料科技有限公司。
聚醚多元醇的羟值为365~395mgKOH/g,官能度为4.2,25℃黏度为2000~3000mpa·s,水分含量≤0.1wt%;优选为INOVOL R6205,由山东一诺威新材料有限公司生产。
交联剂为三官能度小分子醇;优选为甘油或三乙醇胺(TEA)。
匀泡剂A为聚硅氧烷-氧化烯烃嵌段共聚物,优选为美国Air Products公司生产的DC6070和DC2525。
匀泡剂B为硅酮表面活性剂,优选为迈图有机硅材料(上海)有限公司生产的泡沫稳定剂L-580。
催化剂为胺类催化剂或有机金属催化剂,优选为叔胺类催化剂,进一步优选为浓度33wt%的三乙烯二铵、N,N’-二甲基苄胺、2-羟基-N,N,N-三甲基-1-丙胺的甲酸盐按质量比1:(1~2.0):(0.5~1.0)混合而成的复合催化剂。
填料为滑石粉或重质碳酸钙,目数≥600目。
本发明所述的生物基聚氨酯泡沫的制备方法,包括以下步骤:
(1)将木质素、聚己内酯、聚醚多元醇、交联剂、匀泡剂A、匀泡剂B、水、催化剂、填料在常温下混合均匀,得到A组分;
(2)将A组分和B组分按质量比1:1.0~1.5进行混合发泡,即得生物基聚氨酯泡沫。
本发明采用生物可降解木质素、聚己内酯多元醇,交联剂混合在一起,与异佛尔酮二异氰酸酯反应得到的聚氨酯泡沫具有高吸水性,高开孔率及一定的机械强度。
本发明骨架结构中酯键通过水解作用分解为醇和羧酸,氨基甲酸酯键在水解作用下分解为氨基甲酸和醇。采用异佛尔酮二异氰酸酯骨架结构中不含苯环基团,环状烷烃链在自然环境作用下较易断链分解。根据磷酸盐缓冲液水解试验法,确定该发明的聚氨酯泡沫降解速率较聚醚型聚氨酯泡沫具有更快的降解速率,对环境更友好。
与现有技术相比,本发明具有以下有益效果:
(1)本发明制备的聚氨酯泡沫具有可生物降解性,在用于切花泥材料及无土栽培基质使用后,经过掩埋3-5年可生物降解,分解后的有机物小片段,进而分解为二氧化碳和水,对环境友好;
(2)本发明制备的聚氨酯泡沫具有高吸水性,高开孔率及一定的机械强度,适用于仿生土壤,插花泥等领域;
(3)本发明采用水作为发泡剂,其臭氧消耗潜值(ODP)为零,全球变暖潜值(GWP)较低,安全环保的特点;
(4)本发明的组合料,符合聚氨酯泡沫手工操作及机器批量化生产的工艺要求,具有较高的可操作性。
具体实施方式
以下结合实施例对本发明做进一步描述。
实施例1
(1)A组分:木质素45%,聚己内酯(PCL205)27%,INOVOL R6205 15%,甘油5%,泡沫稳定剂DC6070 1%,表面活性剂L-580 1%,复合催化剂(浓度33wt%的三乙烯二铵、N,N’-二甲基苄胺、2-羟基-N,N,N-三甲基-1-丙胺的甲酸盐按质量比1:1.5:0.8混合)0.7%,H2O5.3%。
根据上述配方,将各组分按照比例加入不锈钢釜内进行混合,常温下以120r/min的转速搅拌0.5h,放料作为A组分。
(2)B组分:异佛尔酮二异氰酸酯(IPDI)。
(3)将A、B组分按质量比1:1.3于22℃下混合,在4000r/min的转速下搅拌8s,置于30cm×30cm×10cm的方模,模具温度设定在45℃,30min开模后室温熟化72h,即得生物基聚氨酯泡沫。
实施例2
(1)A组分:木质素30%,聚己内酯(PCL205)20%,INOVOL R6205 15%,甘油4.5%,泡沫稳定剂DC6070 2%,复合催化剂(浓度33wt%的三乙烯二铵、N,N’-二甲基苄胺、2-羟基-N,N,N-三甲基-1-丙胺的甲酸盐按质量比1:1.5:1混合)1.5%,H2O 12%,滑石粉15%。
根据上述配方,将各组分按照比例加入不锈钢釜内进行混合,常温下以120r/min的转速搅拌0.5h,放料作为A组分;由于A组分中加入填料(滑石粉),故在配制完成后应立即使用,或在生产时按照确定比例加入滑石粉得到制品。
(2)B组分:异佛尔酮二异氰酸酯(IPDI)。
(3)将A、B组分按质量比1:1.3于22℃下混合,在4000r/min的转速下搅拌8s,置于30cm×30cm×10cm的方模,模具温度设定在45℃,30min开模后室温熟化72h,即得生物基聚氨酯泡沫。
实施例3
(1)A组分:木质素30%,聚己内酯(PCL205)20%,INOVOL R6205 15%,甘油5%,泡沫稳定剂DC6070 2%,复合催化剂(浓度33wt%的三乙烯二铵、N,N’-二甲基苄胺、2-羟基-N,N,N-三甲基-1-丙胺的甲酸盐按质量比1:1.5:0.8混合)2%,H2O 12%,重质碳酸钙15%。
根据上述配方,将各组分按照比例加入不锈钢釜内进行混合,常温下以120r/min的转速搅拌0.5h,放料作为A组分;由于A组分中加入填料(重质碳酸钙),故在配制完成后应立即使用,或在生产时按照确定比例加入重质碳酸钙得到制品。
(2)B组分:异佛尔酮二异氰酸酯(IPDI)。
(3)将A、B组分按质量比1:1.3于22℃下混合,在4000r/min的转速下搅拌8s,置于30cm×30cm×10cm的方模,模具温度设定在45℃,30min开模后室温熟化72h,即得生物基聚氨酯泡沫。
对比例1
(1)A组分:聚醚多元醇INOVOL 330N(羟值33~35mgKOH/g,25℃黏度800~1000mpa·s,水分含量≤0.1wt%)60%,聚醚多元醇INOVOL R6205 15%,聚醚多元醇INOVOL C210(羟值109~115mgKOH/g,25℃黏度120~180mpa·s,水分含量≤0.1wt%)13%,甘油4.5%,泡沫稳定剂DC6070 1%,表面活性剂L-580 1%,复合催化剂(浓度33wt%的三乙烯二铵、N,N’-二甲基苄胺、2-羟基-N,N,N-三甲基-1-丙胺的甲酸盐按质量比1:1.5:0.8混合)0.6%,H2O 4.9%。
根据上述配方,将各组分按照比例加入不锈钢釜内进行混合,常温下以120r/min的转速搅拌0.5h,放料作为A组分。
(2)B组分:异氰酸酯PM200(万华化学股份有限公司)。
(3)将A、B组分按质量比1:1.3于22℃下混合,在4000r/min的转速下搅拌8s,置于30cm×30cm×10cm的方模,模具温度设定在45℃,30min开模后室温熟化72h,即得生物基聚氨酯泡沫。
对比例2
(1)A组分:聚醚多元醇INOVOL 330N 37%,聚醚多元醇INOVOL R6205 15%,聚醚多元醇INOVOL C210 13%,甘油5%,泡沫稳定剂DC6070 2%,复合催化剂(浓度33wt%的三乙烯二铵、N,N’-二甲基苄胺、2-羟基-N,N,N-三甲基-1-丙胺的甲酸盐按质量比1:1.5:0.8混合)1.5%,H2O 11.5%,滑石粉15%。
根据上述配方,将各组分按照比例加入不锈钢釜内进行混合,常温下以120r/min的转速搅拌0.5h,放料作为A组分;由于A组分中加入填料(滑石粉),故在配制完成后应立即使用,或在生产时按照确定比例加入滑石粉得到制品。
(2)B组分:异氰酸酯PM200(万华化学股份有限公司)。
(3)将A、B组分按质量比1:1.3于22℃下混合,在4000r/min的转速下搅拌8s,置于30cm×30cm×10cm的方模,模具温度设定在45℃,30min开模后室温熟化72h,即得生物基聚氨酯泡沫。
实施例1、对比例1所制得的聚氨酯泡沫应用于仿生土壤材料,实施例2-3、对比例2所制得的聚氨酯泡沫应用于插花泥材料。
将实施例1-3和对比例1-2制备的聚氨酯泡沫进行性能检测。其中降解性能表征采用户外土埋降解实验法进行:对实施例1-3和对比例1-2制备的聚氨酯泡沫编号为A、B,C,D和E,称量其重量为m0,按一定间隔埋入普通园艺土壤下约10cm处,让其在自然条件下降解90天后取出生物基聚氨酯泡沫样品,用去离子水清洗,然后在50℃鼓风干燥箱中放置24h进行干燥,最后在常温条件下平衡24h,再次称量其重量为m1,计算泡沫的失重率(失重率=(m0-m1)/m0×100%)。
性能检测结果见表1。
表1实施例1-3及对比例1-2聚氨酯泡沫性能检测结果
性能指标 实施例1 实施例2 实施例3 对比例1 对比例2
泡沫芯密度,kg/m<sup>3</sup> 35.2 36.5 36.2 35.3 36.4
泡沫开孔率,% 68 72 73 67 70
泡沫吸水率,% 458 621 684 386 493
失重率,%(90天) 9.8 11.2 11.3 0.4 0.7
压缩强度,kPa 117 154 159 121 160
从表1可以看出,本发明制备的聚氨酯泡沫具有高吸水性,高开孔率及一定的机械强度,适用于仿生土壤,插花泥等领域;对比例1-2采用常规配方制备聚氨酯泡沫,在泡沫密度和开孔率相当的条件下,泡沫的吸水率明显降低,其生物降解性也较差。

Claims (9)

1.一种生物基聚氨酯泡沫,其特征在于:由A组分和B组分按质量比1:1.0~1.5混合制成;
以质量百分数计,A组分由以下原料组成:
木质素 30~60%
聚己内酯 20~30%
聚醚多元醇 10~20%
交联剂 3~5%
匀泡剂A 1~2%
匀泡剂B 1~2%
水 0.5~10%
催化剂 0.3~1.5%
填料 0~20%;
B组分为异佛尔酮二异氰酸酯;
聚己内酯的羟值为200~240mgKOH/g,官能度为2,30℃黏度为250~350mpa·s,水分含量≤0.05wt%。
2.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:木质素的熔点为154~162℃。
3.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:聚醚多元醇的羟值为365~395 mgKOH/g,官能度为4.2,25℃黏度为2000~3000mpa·s,水分含量≤0.1wt%。
4.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:交联剂为三官能度小分子醇。
5.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:匀泡剂A为聚硅氧烷-氧化烯烃嵌段共聚物。
6.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:匀泡剂B为硅酮表面活性剂。
7.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:催化剂为胺类催化剂或有机金属催化剂。
8.根据权利要求1所述的生物基聚氨酯泡沫,其特征在于:填料为滑石粉或重质碳酸钙,目数≥600目。
9.一种权利要求1-8任一项所述的生物基聚氨酯泡沫的制备方法,其特征在于:包括以下步骤:
(1)将木质素、聚己内酯、聚醚多元醇、交联剂、匀泡剂A、匀泡剂B、水、催化剂、填料在常温下混合均匀,得到A组分;
(2)将A组分和B组分按质量比1:1.0~1.5进行混合发泡,即得生物基聚氨酯泡沫。
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