CN113956635B - 一种可生物降解聚酯组合物及其应用 - Google Patents
一种可生物降解聚酯组合物及其应用 Download PDFInfo
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- CN113956635B CN113956635B CN202011409013.6A CN202011409013A CN113956635B CN 113956635 B CN113956635 B CN 113956635B CN 202011409013 A CN202011409013 A CN 202011409013A CN 113956635 B CN113956635 B CN 113956635B
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- polyester resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及可生物降解聚酯领域,具体的更涉及一种可生物降解聚酯组合物及其应用。一种可生物降解聚酯组合物,包括颜料、可降解聚酯树脂、功能添加剂、填料、助剂;其中,所述可降解聚酯树脂包括(a)聚乳酸和(b)脂肪族/芳香族混合聚酯树脂,以组合物的总重量为基准,可降解聚酯树脂在组合物中的含量为50~90%。
Description
技术领域
本发明涉及可生物降解聚酯领域,具体的更涉及一种可生物降解聚酯组合物及其应用。
背景技术
可生物降解聚酯由石油提炼加工合成,对比传统石油基材料,可生物降解聚酯在堆肥和自然填埋情况下可分解成二氧化碳和水,不会造成白色污染。可生物降解聚酯着色母粒为可生物降解聚酯提供不同的颜色,降解后不会为土壤带来重金属和其他的二次污染。堆肥可生物降解聚酯的肥料和填埋可生物降解聚酯的土地,可直接使用,不用再经过处理。
可生物降解聚酯广泛应用于快递袋、购物袋、厨余垃圾袋、食品包装膜、农用地膜等领域。但是,在着色过程中没选好颜料助剂会导致堆肥或填埋后重金属超标;此外现有的专利比如CN1368516、CN101392078、CN101319068等采用聚乙烯或乙烯醋酸乙烯共聚物等不可降解材料为载体,这必然影响到产品的最终降解性能。中国专利CN101475695和CN102040814虽然采用生物可降解塑料为载体,然而这些专利中也添加了聚乙烯蜡、氧化聚乙烯蜡或EBS等不可降解助剂,制备得到的色母粒在降解时对作物产量有影响。中国专利CN102391626中选用的载体树脂虽然为生物基可完全降解聚合物,但是该专利中未添加任何加工助剂,这导致色母粒在生产过程中颜料分散效果不理想、加工粘度较大、后续使用容易出现色点等问题。
发明内容
除非另有说明、从上下文暗示或属于现有技术的惯例,否则本申请中所有的份数和百分比都基于重量,且所用的测试和表征方法都是与本申请的提交日期同步的。如果现有技术中披露的具体术语的定义与本申请中提供的任何定义不一致,则以本申请中提供的术语定义为准。
本发明中的词语“优选的”、“优选地”、“更优选的”等是指,在某些情况下可提供某些有益效果的本发明实施方案。然而,在相同的情况下或其他情况下,其他实施方案也可能是优选的。此外,对一个或多个优选实施方案的表述并不暗示其他实施方案不可用,也并非旨在将其他实施方案排除在本发明的范围之外。本发明中未提及的组分的来源均为市售。
本发明人为了解决上述问题经过认真研究后发现,通过在特定的可降解聚酯树脂引入功能添加剂实现一定的交联的同时可以提高组合物的强度和韧性,以及十分有益的堆肥效果。
本发明第一个方面提供了一种可生物降解聚酯组合物,包括颜料、可降解聚酯树脂、功能添加剂、填料、助剂;其中,所述可降解聚酯树脂包括(a)聚乳酸和(b)脂肪族/芳香族混合聚酯树脂,以组合物的总重量为基准,可降解聚酯树脂在组合物中的含量为30~80%,优选40~70%。
<颜料>
作为颜料包括无机和有机颜料,可以是《化工产品手册:颜料》中所记载的一般的无机颜料或有机颜料。
作为无机颜料,可以列举钛白、钛黄等含钛的(复合)金属氧化物、氧化锌、氧化铁、炭黑、群青、硫化锌、三氧化锑等;作为有机颜料,可以列举酞菁类颜料、蒽醌类颜料、喹吖啶酮类颜料、偶氮类颜料、异吲哚啉酮类颜料、喹酞酮类颜料、紫环酮类颜料、苝类颜料等颜料。以上颜料可以单独使用,也可以混合使用,其中,以组合物的总重量为基准,颜料的含量为20~50%,优选20~35%。
适合本发明的颜料,特别优选钛白粉、炭黑、群青、酞青、有机黄中的至少一种,在这些颜料中,为获得更好的堆肥效果,优选吸油值在5~50g/100g或30~75m2/kg之间的颜料,更优选吸油值在10~50g/100g或50~65m2/kg之间,吸油值越高,浸润颜料表面孔隙所需的油量越多,则在颜料一定时润湿分散剂的含量必然较高,引入较多的有机污染物影响堆肥。
<可降解聚酯树脂>
作为可降解聚酯树脂,优选包括(a)聚乳酸和(b)脂肪族/芳香族混合聚酯树脂,以组合物的总重量为基准,所述(a)聚乳酸和(b)脂肪族/芳香族混合聚酯树脂的质量比(a):(b)=1:5~5:1,优选1:3~3:1,更优选1:2~2:1。
作为(a)聚乳酸可以仅使用一种树脂或以两种以上树脂的组合使用,可以是L-乳酸的均聚物或D-乳酸的均聚物,或L-乳酸和D-乳酸的共聚物。适合的L-乳酸和D-乳酸的共聚物可以是由例如20~100mol%L-乳酸单元或D-乳酸单元和0~80mol%相应的对映体(旋光异构体)单元构成的共聚物。
此外,作为(a)聚乳酸还可以是立体络合物聚乳酸,例如由聚乳酸(A)和聚乳酸(B)的混合物构成且(A)/(B)(质量比)为10/90~90/10,聚乳酸(A)由90~100mol%L-乳酸单元和0~10mol%D-乳酸单元组成,聚乳酸(B)由90~100mol%D-乳酸单元和0~10mol%L-乳酸单元组成。构成立体络合物聚乳酸的各聚乳酸(A)和(B)中除了乳酸之外的共聚成分包括具有两个以上各自能够形成酯键的官能团的二羧酸、多元醇、羟基羧酸、内酯等。
通过对上述(a)聚乳酸的研究,适合的(a)聚乳酸优选重均分子量大于50000的聚乳酸,可以是单一分子量的聚乳酸,也可以是不同分子量混合的聚乳酸。更优选的,聚乳酸为重均分子量大于50000的双轴取向聚合物,此类聚乳酸包括NatureWorks6201D、6202D、6251D、3051D,这些聚乳酸可以单独使用,也可以混合使用;其中,特别优选的是4044D和/或4043D,最优选4043D。4043D是密度在1.24g/cm3,熔体质量流动速率(210度,2.16kg)为6.0g/10min的双轴取向聚合物。
聚合物的取向一般有单轴取向和双轴取向两种方式。单轴取向指在一个轴向上施以外力,使分子链沿一个方向取向;对应的,双轴取向指在两个垂直方向施加外力,使分子链取向平行薄膜平面的任意方向。经过取向后的分子结晶度提高,比如双轴取向的聚乳酸结晶度高于单轴取向的结晶度,因此双轴取向聚乳酸在各方向上的强度更高,但断裂伸长率下降。
在研究中考虑到双轴取向聚乳酸的断裂伸长率与其拉伸强度之间难以平衡,意外发现通过与(b)脂肪族/芳香族混合聚酯树脂相互协同,尤其是优选为以脂肪族二醇、脂肪族二羧酸和芳香族二羧酸作为主要原料得到的脂肪族/芳香族混合聚酯树脂能在保持力学性能的同时保证一定的堆肥效果。
这里的脂肪族二醇优选具有3~10个碳原子的脂肪族二醇,特别优选具有4~6个碳原子的脂肪族二醇。具体地说,包括1,3-丙二醇、1,4-丁二醇、1,4-环己二甲醇等,其中特别优选1,4-丁二醇。
这里的脂肪族二羧酸和芳香族二羧酸中的二羧酸优选为具有3~10个碳原子的二羧酸。具体地说,包括丁二酸、己二酸、辛二酸、癸二酸、对苯二酸等,其中特别优选丁二酸、己二酸、对苯二甲酸,最优选己二酸、对苯二甲酸。
通过对上述(b)脂肪族/芳香族混合聚酯树脂的研究,适合的(b)脂肪族/芳香族混合聚酯树脂为已二酸丁二醇酯和对苯二甲酸丁二醇酯的共聚物,是一种热塑性生物降解柔性塑料。
在对脂肪族/芳香族混合聚酯树脂的研究中,优选密度在1.25~1.35g/cm3之间,熔体质量流动速率(210度,2.16kg)在2.0~5.0g/10min之间的脂肪族/芳香族混合聚酯树脂,作为此类树脂包括新疆蓝山屯河的THJS系列,例如THJS-6802、THJS-7801、THJS-8801、THJS-5801、THJS-6801。
THJS系列具有适宜的脂肪链以及芳香结构,脂肪链段具有与聚乳酸相似的结构,因此加入到聚乳酸中促进了聚乳酸分子链的迁移,起到了一定的成核作用,在加工过程中进一步提高取向。在降解时,THJS系列脂肪族/芳香族混合聚酯树脂的存在因位阻比聚乳酸中酯基更难被水分子降解,所以导致降解先从取向性的降解再到非取向性降解,从而使整体的降解速率达到均衡,因此在整个堆肥中都不会产生不良影响,对作物有非常好的堆肥效果。
<功能添加剂>
作为功能添加剂,优选至少含有1个环氧基团的环氧类物质,通过引入环氧基团和上述优选的聚乳酸的端基,例如聚乳酸中的羟基或羧基反应,可以扩充直链或支链,从而改善无机填料的分散性以及组合物的力学性能。
作为优选,至少含有1个环氧基团的环氧类物质选自环氧烷烃、缩水甘油酯、环氧类丙烯酸共聚物中的至少一种。
作为环氧烷烃例如可列举出环氧乙烷、环氧丙烷、1,2-环氧丁烷、1,4-环氧丁烷、1,4-二氧六环、二环氧基的长链烷烃化合物、以及上述的化合物被任意卤素取代的环氧烷烃,其中,二环氧基的长链烷烃化合物例如包括1,7-辛二烯二环氧化合物等。
作为缩水甘油酯例如可列举出新癸酸缩水甘油酯、异氰尿酸三缩水甘油酯、叔碳酸缩水甘油酯、六氢邻苯二甲酸二缩水甘油酯等,其中较好的是叔碳酸缩水甘油酯,例如包括新戊酸缩水甘油酯、新庚酸缩水甘油酯、新壬酸缩水甘油酯、新癸酸缩水甘油酯、新十一酸缩水甘油酯、新十三酸缩水甘油酯。
作为环氧类丙烯酸共聚物通常是在环氧树脂与不饱和一元酸反应得到的环氧丙烯酸酯中,使用聚合性乙烯基单体作为反应性稀释剂的树脂。作为这类的环氧类丙烯酸共聚物可以列举出:将以双酚A、双酚F、以及溴化双酚A为代表的双酚化合物作为主骨架的二环氧甘油醚型环氧树脂等;将以苯酚、甲酚酚醛、溴化的苯酚酚醛为代表的多核苯酚化合物作为骨架的聚缩水甘油醚型环氧树脂等;将以二聚酸、偏苯三酸为代表的有机多元酸作为主骨架的聚缩水甘油酯型环氧树脂等;将以双酚A环氧乙烷、加成环氧丙烷的乙二醇以及加氢的双酚A化合物作为骨架的缩水甘油醚型环氧树脂等。具体地说,更优选环氧树脂TDE-85、E-20、E-44、E-51,最优选同时含有脂环族环氧基和缩水甘油酯基的三官能团环氧树脂TDE-85。
作为适合本发明的功能添加剂优选包括上述的缩水甘油酯和环氧类丙烯酸共聚物;作为功能添加剂之一的缩水甘油酯可以单独使用,也可以任意两种或以上混合使用,作为功能添加剂之一的环氧类丙烯酸共聚物可以单独使用,也可以任意两种或以上混合使用,优选以组合物的总重量为基准,功能添加剂的总含量占组合物为1~10%,优选2~8%,更优选2~5%。
通过对上述功能添加剂的研究进一步优选出,包括(c)叔碳酸缩水甘油酯以及(d)从环氧树脂TDE-85、E-20、E-44、E-51中选出的至少一种;尤其优选的是包括(c)叔碳酸缩水甘油酯以及(d)环氧树脂TDE-85的功能添加剂,两者的添加浓度可以在相对较宽的范围内存在,优选(c):(d)=1:5~5:1,优选1:3~3:1,更优选1:2~2:1。
这些环氧物质的功能添加剂中,环氧树脂TDE-85具有缩水甘油酯基和酯环环氧基,同时分子中的两类环氧基具有不同的反应活化能,活化能低的缩水甘油酯基与叔碳酸的缩水甘油酯先与聚乳酸以及聚酯上的羧基和羟基迅速反应,生成的羟基被缩水甘油酯进一步反应后在树脂中交联聚集,而活化能较高的酯环环氧基在反应中与这些交联聚集体之间连接成均匀分散的核交联结构提高力学性。
叔碳酸的缩水甘油酯中具有高度支化的含有较大的疏水性长链结构,在研究中发现通过将其与环氧树脂一起可被引入树脂中,解决了基体相容性问题。而进一步由于叔碳酸的多支链化结构还能降低树脂基体的粘度,同时提高颜料的润湿性使其更好的被分散。尤其是当其反应完后生成的大量的羟基官能团能促进交联。
<填料>
作为填料优选无机填料,填充以改善耐热性和刚度。无机填料包括但不限于滑石粉、碳酸钙、硫酸钙、氧化镁、硬脂酸钙、硅灰石、云母、二氧化硅、硅酸钙、粘土和炭黑。在这些无机填料中,优选硅灰石和滑石粉。最优选平均颗粒度0.5-10μm,优选5~10μm的滑石粉。其中,以组合物的总重量为基准,填料的含量为5~30%,优选5~20%;如果含量在此范围以外,就很难改善耐热性和刚度。
<助剂>
本发明的组合物中,在不有损本发明的期望的效果的范围内,可以配混通常一般使用的添加剂。作为添加剂,例如可以举出:润滑剂、阻燃剂、抗氧剂、紫外线吸收剂等。这些添加剂可以含有在本发明的组合物中,也可以与本发明的组合物分开地添加至实际产品中。
作为润滑剂,例如可以列举脂肪族羧酸金属盐、脂肪族羧酸酯、脂肪族羧酸、烃系化合物、石蜡、酮化合物、羧酰胺、双酰胺化合物等,其中,优选脂肪族羧酸金属盐、脂肪族羧酸酯、烃系化合物、酮化合物,更优选脂肪族羧酸金属盐、脂肪族羧酸酯。
脂肪族羧酸金属盐优选是碳数16~36的高级脂肪酸的金属盐,例如可以列举硬脂酸镁、硬脂酸钙、硬脂酸钡、褐煤酸钙、褐煤酸钠、硬脂酸锌、硬脂酸铝、硬脂酸钠、硬脂酸锂等。
脂肪族羧酸酯是指,由脂肪族羧酸和醇形成的化合物,例如可以列举蜂蜡、羊毛脂、硬脂酸硬脂酸酯、山嵛酸山嵛酸酯、硬脂酸山嵛酸酯、甘油单棕榈酸酯、甘油单硬脂酸酯、甘油二硬脂酸酯、甘油三硬脂酸酯、季戊四醇单棕榈酸酯、季戊四醇单硬脂酸酯、季戊四醇二硬脂酸酯、季戊四醇三硬脂酸酯、季戊四醇四硬脂酸酯。
通常在使用上述润滑剂的情况下,以组合物的总重量为基准,润滑剂的含量为1~10%,优选3~8%。
作为阻燃剂,例如可以列举磷类阻燃剂,例如磷酸酯、膦酸酯和磷化物[例如磷酸三甲苯酯、磷酸三(2,3-二溴丙基)酯、二甲基甲烷膦酸酯、多聚磷化物和多磷酸铵]、以及红磷;含有卤素的阻燃剂,例如溴类阻燃剂(有机溴化合物,例如十溴二苯醚和四溴双酚A)、以及氯类阻燃剂(例如六氯桥亚甲基四氢化邻苯二甲酸(HET acid));金属(氢)氧化物,例如三氧化锑、氢氧化镁和氢氧化铝;以及硼酸盐类阻燃剂,例如硼酸锌和偏硼酸钡。通常在使用上述阻燃剂的情况下,以组合物的总重量为基准,阻燃剂的含量为1~10%,优选3~8%。
作为抗氧化剂,例如可以列举酚类(受阻酚),例如2,6-二叔丁基对甲酚(BHT)和2,2’-亚甲基双(4-甲基-6-叔丁基苯酚);硫类,例如3,3’-硫代二丙酸二月桂酯(DLTDP)和二硬脂酰3,3’-硫代二丙酸酯(DSTDP);磷类(选择性地具有卤素的有机磷化物),例如三苯基磷化物(TPP)、三异癸基磷化物(TDP)、以及它们的卤代物;以及胺类(受阻芳香族胺),例如辛基二苯基胺、N-正丁基对氨基苯酚和N,N-二异丙基对亚苯基二胺。通常在使用上述抗氧化剂的情况下,以组合物的总重量为基准,抗氧化剂的含量为1~10%,优选3~8%。
作为紫外线吸收剂,例如可以列举二苯甲酮类,例如2-羟基二苯甲酮和2,4-二羟基二苯甲酮;水杨酸酯类,例如水杨酸苯酯和2,4-二叔丁基苯基-3,5-二叔丁基-4-羟基苯甲酸酯;苯并三唑类,例如(2’-羟苯基)苯并三唑和(2’-羟基-5’-甲苯基)苯并三唑;以及丙烯酸类,例如乙基-2-氰基-3,3’-二苯基丙烯酸酯和甲基-2-甲氧甲酰基-3-(对甲氧基苄基)丙烯酸酯。通常在使用上述紫外线吸收剂的情况下,以组合物的总重量为基准,紫外线吸收剂的含量为1~10%,优选3~8%。
本发明第二个方面提供了上述组合物在着色母粒中的应用,通常情况下本发明的组合物可以单独制作着色母粒,又或者可以复合具有一定功能的其他物质共同制作着色母粒,例如在实际供应过程中针对客户的需求可进行定制特定功能的着色母粒,这里定制中添加的其他组分可以是增韧物质、耐磨物质、营养物质等等。
着色母粒的制备过程可采用常规制作方法,例如按比例混合各物料后投入双螺杆挤出机中,于150-190℃挤出、造粒即可得到。母粒的大小可以是任意大小,也可依据实际需求进行调整,本发明对此不作任何限定。通常在获得堆肥效果的母粒的平均粒度可以为0.1~3mm。作为着色母粒可以以2%~5%的添加量与各种塑料基体进行混合得到吹膜管材、餐盒、地膜等等。
附图说明
图1:实施例1~5的组合物得到的着色母粒
图2:7天潜伏期(从下到上)后大麦植物生长情况,下:25%空白堆肥,上:25%测试堆肥
图3:7天潜伏期(从下到上)后大麦植物生长情况,下:50%空白堆肥,上:50%测试堆肥
具体实施方式
下面通过实施例对本发明进行具体的描述,以下实施例只能用于本发明做进一步说明,并不能理解为本发明保护的限制,该领域的专业技术人员根据上述发明的内容作出的非本质的改正和调整,仍属于本发明的保护的范围。
实施例1
可生物降解聚酯组合物(R1白色)的组成见下表:
表1
原料名称 | 重量(单位:克) |
金红石型钛白粉(LR-108,吸油值13-17g/100g) | 25 |
聚乳酸(4043D) | 34 |
脂肪族/芳香族混合聚酯树脂(THJS-6802) | 22 |
新壬酸缩水甘油酯 | 1 |
环氧树脂(TDE-85) | 1.6 |
滑石粉 | 11 |
油酸酰胺 | 3.8 |
乙撑双硬脂酰胺 | 1.6 |
实施例2
可生物降解聚酯组合物(R2黑色)的组成见下表:
表2
实施例3
可生物降解聚酯组合物(R3绿色)的组成见下表:
表3
原料名称 | 重量(单位:克) |
金红石型钛白粉(LR-108,吸油值13-17g/100g) | 15 |
颜料黄(2927,吸油值34g/100g) | 9 |
酞菁蓝B(吸油值45g/100g) | 1 |
聚乳酸(4043D) | 34 |
脂肪族/芳香族混合聚酯树脂(THJS-8801) | 22 |
新戊酸缩水甘油酯 | 1 |
环氧树脂(TDE-85) | 1.6 |
滑石粉 | 11 |
油酸酰胺 | 3.8 |
乙撑双硬脂酰胺 | 1.6 |
实施例4
可生物降解聚酯组合物(R4蓝色)的组成见下表:
表4
原料名称 | 重量(单位:克) |
金红石型钛白粉(LR-108,吸油值13-17g/100g) | 20 |
巴斯夫L7460酞菁蓝(吸油值45g/100g) | 5 |
聚乳酸(4043D) | 34 |
脂肪族/芳香族混合聚酯树脂(THJS-6802) | 22 |
新庚酸缩水甘油酯 | 1 |
环氧树脂(TDE-85) | 1.6 |
滑石粉 | 11 |
油酸酰胺 | 3.8 |
乙撑双硬脂酰胺 | 1.6 |
实施例5
可生物降解聚酯组合物(R5黄色)的组成见下表:
表5
原料名称 | 重量(单位:克) |
金红石型钛白粉(LR-108,吸油值13-17g/100g) | 13 |
颜料黄(2927,吸油值34g/100g) | 12 |
聚乳酸(4043D) | 34 |
脂肪族/芳香族混合聚酯树脂(THJS-6801) | 22 |
新壬酸缩水甘油酯 | 1 |
环氧树脂(TDE-85) | 1.6 |
滑石粉 | 11 |
油酸酰胺 | 3.8 |
乙撑双硬脂酰胺 | 1.6 |
实施例6
可生物降解聚酯组合物(R6白色)的组成见下表:
表6
原料名称 | 重量(单位:克) |
金红石型钛白粉(LR-108,吸油值13-17g/100g) | 25 |
聚乳酸(4043D) | 56 |
新壬酸缩水甘油酯 | 1 |
环氧树脂(TDE-85) | 1.6 |
滑石粉 | 11 |
油酸酰胺 | 3.8 |
乙撑双硬脂酰胺 | 1.6 |
实施例7
可生物降解聚酯组合物(R7白色)的组成见下表:
表7
实施例8
可生物降解聚酯组合物(R8白色)的组成见下表:
表8
原料名称 | 重量(单位:克) |
金红石型钛白粉(LR-108,吸油值13-17g/100g) | 25 |
聚乳酸(4043D) | 34 |
脂肪族/芳香族混合聚酯树脂(THJS-6802) | 22 |
环氧丙烷 | 1 |
环氧树脂(TDE-85) | 1.6 |
滑石粉 | 11 |
油酸酰胺 | 3.8 |
乙撑双硬脂酰胺 | 1.6 |
1.1力学性能测试
通过将实施例1~8制成母粒,与PPC按照1:5得到的农用地膜的力学性能按GB13735-92标准检测,其中实施例1~5的拉伸强度≥10MPa,断裂伸长率≥90%,直角撕裂负荷≥40KN/M,为合格产品;实施例6的断裂伸长率<90%,不合格;实施例7、8的直角撕裂负荷<40KN/M;不合格。
1.2挥发性固体含量
通过将实施例1~5在105℃下干燥至少14小时来确定总固体或干物质含量,结果以百分比给出,结果见下表1,均满足对挥发性固体的要求以及ASTM D6400(2012)和CAN/BNQ 0017-088(2010)定义的重金属要求,结果见下表2。
表1
表2
1.3堆肥实验
1.3.1实验方法
大麦植物生长试验在500毫升个花盆中进行,其中包含堆肥和参考基质的混合物。每种堆肥在2种堆肥和参考基质的混合比中进行测试:(1)75%种参考基质和25%种堆肥,以及(2)50%种参考基质和50%种按重量计算的堆肥。每种混合物在3次重复中进行测试。在测试开始时,每个花盆填充至少200克堆肥/参考基质混合物,并加入100毫升的软化水。随后,将50个大麦种子放在混合物的顶部,并用薄层硅质砂覆盖。最后,可以添加额外量的软化水以确保最佳水分含量。花盆完全准备好后,用玻璃板覆盖它们,并在黑暗中在20℃ 2℃的恒定温度下孵育。发芽后,取出平板,并在每天至少12小时内将花盆暴露于至少3000勒克斯的光强度。在测试过程中,如果需要,额外加水,并记录视觉感知。为了避免副作用,在测试期间,根据逻辑旋转方案改变每个锅的位置。测试在11(±1)天后完成。在测试结束时,分别为每个花盆确定上述土壤植物材料的总新鲜和干重。还测量了发芽率。通过比较测试堆肥和空白堆肥的发芽和植物产量的结果,评估了测试项目可能残留的毒性。
1.3.2空白和测试堆肥的组成
表3
空白堆肥(G湿重) | 测试堆肥(G湿重) | 测试堆肥(G干重) | 干测试项目百分比 | |
成熟堆肥 | 1750.00 | 1744.18 | 880.81 | - |
R5黄色 | - | 3.98 | 3.88 | 0.22 |
R4蓝色 | - | 1.94 | 1.94 | 0.11 |
1.3.3分析方法
(1)铵氮(NH4+-N)含量;依据国际汽联法测定氨氮(光谱检测)。铵-N在水提取物中测定。含有铵离子的样品通过注入阀注入到连续的载流子流中,并与碱性溶液的连续流流混合。形成的气态氨通过扩散池从疏水半渗透膜上的溶液中分离出来,并被包含pH指示剂的流动受体流吸收。由于产生的pH偏移,指示剂溶液将改变其颜色,该颜色在590nm的流动光度计中连续测量。结果以g/l湿重为单位给出。
(2)发芽能力:将5毫升的软化水加入到培养皿中,滤纸放在棉花层的顶部。将二十个大麦种子放在滤纸上。第二张滤纸放在种子上。培养皿用parafilm密封,并在室温下置于黑暗中。5天后,计算发芽种子的数量。发芽以开始时种子量的%为单位。5次重复测试发芽能力。
(3)硝酸盐和亚硝酸盐氮含量:依据FIA法测定总氧化氮(光谱检测)”.测定是在水提取物上进行的。通过注入阀将含有亚硝酸盐/硝酸盐离子的样品送入连续流动的缓冲溶液(载体流)中。样品中的硝酸盐在镉还原剂中还原为亚硝酸盐。在添加酸性磺胺酰胺溶液时,亚硝酸盐最初存在,硝酸盐还原形成的亚硝酸盐将形成重氮化合物。该化合物与N-(1-naphtyl)-乙二胺二盐酸盐(NED)偶联形成紫色偶氮染料。这种偶氮染料在540纳米处测量。结果以g/l湿重为单位给出。
(4)总氮(N):该分析按照“冰毒l.005”中的描述进行。总氮的测定。在催化剂的存在(K2所以4-混合物)和沸腾条件下(380℃-395℃)与硫酸-水杨酸结合的氮混合物转化为盐(NH4)2所以之后,使用强碱释放氨,并通过滴定蒸馏进行后续测定。氨在硼酸/指示剂溶液中被捕获。馏出物中铵离子的测定是通过用标准酸滴定来完成的。结果以g/kg总固体为单位给出。
1.3.4测试条件
测试项目将黄色颜料和蓝色颜料与成熟堆肥混合,以获得在干重基础上分别为0.22%和0.11%的特定浓度。这些浓度基于可堆肥材料中的最大浓度分别为0.8%和0.4%(基于干重)并且假设在堆肥试验开始时将可堆肥材料以10%的浓度添加到生生物废物中,并在堆肥试验结束时降解90%。在堆肥过程中,只有部分原始废物(约为生物废物原始重量的35%)和可堆肥材料最终会成为最终堆肥(分数<10毫米),而测试项目,在最坏的情况下,将完全在最终的堆肥中结束。因为在正常情况下,测试项目在它们来之前要经过堆肥过程与植物接触时,一个小的并且在58℃下在黑暗中进行7天,在20℃下进行3天的简单稳定过程。注意曝气和含水量。在堆肥过程中,定期搅拌反应器的内容物。在此过程中,测试项目可以部分或完全生物降解。如果没有堆肥,由于生物活性和堆肥的不成熟,测试项目可能对植物产生毒性作用,这并不代表现实。根据EN 13432(2000),ASTM D6400(2012)和ISO 17088(2012),这种稳定性可以持续12周。必须注意的是,稳定期的缩短确实使生态毒性试验更加严格。经过厌氧堆肥超过12周的新鲜预处理的城市固体废物。表4给出了成熟堆肥的特性。在使用之前,将坯料和测试堆肥充分混合。总共使用了12个花盆,参考基质和堆肥的混合物以重量为基础给出,表5描述了测试设置。
表4
类别 | 组成 |
总固体含量(TS%) | 50.5 |
含水量(%) | 49.5 |
挥发性固体(VS,%on TS) | 38.8 |
灰分含量(%on TS) | 61.2 |
pH | 7.8 |
电导率(EC,μS/cm) | 2890 |
NOx --N(mg/l) | 446 |
NH4 +-N(mg/l) | 16 |
Total N(g/kg TS) | 21.8 |
C/N | 9 |
表5
类别 | 参考基质 | 堆肥 |
3份空白堆肥(25%) | 172.5 | 57.5 |
3份空白堆肥(50%) | 115.0 | 115.0 |
3份测试堆肥(25%) | 172.5 | 57.5 |
3份测试堆肥(50%) | 115.0 | 115.0 |
1.4测试结果
发芽和产量:表6表示不同测试系列的平均发芽率占开始时添加的种子总量的百分比。相对发芽率也如图1所示。表6显示了每个测试系列的平均新鲜和干重产量(土壤上植物部分)以及标准偏差。结果如图2和图3所示。作为一般结论,可以说明将浓度为0.8%(干重)的黄色颜料和浓度为0.4%(干重)的蓝色颜料添加到
可堆肥材料中,经过10天的堆肥稳定期后,对大麦植物的出苗和生长没有负面影响。
表6
Claims (5)
1.一种可生物降解聚酯组合物,其特征在于,包括颜料、可降解聚酯树脂、功能添加剂、填料、助剂;其中,所述可降解聚酯树脂包括(a)聚乳酸和(b)脂肪族/芳香族混合聚酯树脂,以组合物的总重量为基准,可降解聚酯树脂在组合物中的含量为50~90%;
所述(a)聚乳酸和(b)脂肪族/芳香族混合聚酯树脂的质量比(a):(b)=1:5~5:1;
所述脂肪族/芳香族混合聚酯树脂为已二酸丁二醇酯和对苯二甲酸丁二醇酯的共聚物;
所述功能添加剂包括叔碳酸缩水甘油酯和环氧树脂TDE-85;
所述功能添加剂的总含量占组合物总重量的1~10%;
所述助剂包括润滑剂、阻燃剂、抗氧剂、紫外线吸收剂中的至少一种。
2.如权利要求1所述的组合物,其特征在于,所述聚乳酸的重均分子量大于50000。
3.如权利要求2所述的组合物,其特征在于,所述聚乳酸为双轴取向聚合物。
4.如权利要求1~3任一项所述的组合物,其特征在于,所述填料的平均粒度为0.5-10μm。
5.如权利要求1~4中任一项所述的组合物在着色母粒中的应用。
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