CN116397440A - 一种含有益生菌微胶囊的功能性植物纤维 - Google Patents
一种含有益生菌微胶囊的功能性植物纤维 Download PDFInfo
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Abstract
本发明公开了一种含有益生菌微胶囊的功能性植物纤维,其制备途径为:在植物叶片制备成纺丝原液纺纱的过程中,添加益生菌微胶囊和增效剂后,通过湿法纺丝制成功能性植物纤维。本发明制备得到的功能性植物纤维不仅具有良好的抑菌功能,还具有良好的防紫外线功能,在服装、家纺等纺织品领域具有良好应用前景。
Description
技术领域
本发明涉及植物纤维生产技术领域,具体涉及一种含有益生菌微胶囊的功能性植物纤维。
背景技术
天然植物纤维是自然界中最为丰富的可再生资源之一,具有生物可降解性和环境友好性的特点,其主要成分纤维素、半纤维素和木素大分子结构中含有能够参与化学反应的官能团,可制备出多种用途的功能性材料,应用于纺织、造纸和复合材料等领域。在我国南方的省份,例如广东、广西、海南等地,广泛种植了香蕉、菠萝等植物,将香蕉茎秆、菠萝叶等农业废弃物作为制备纤维的原料加以利用,避免了以往丢弃在田间或焚烧造成的环境污染和资源浪费,也能带来相应的经济价值,具有良好的研究前景。
随着中国市场经济的繁荣发展和人民生活水平的提高,人们对纺织服装业也提出新的要求,众多企业也都加入到健身护身、防止疾病这一潜力巨大的纺织品新市场。新型特种保健纤维正在不断推出,各种各样的功能性纤维被研发出来,所谓的功能性纤维就是以使纤维获得某种特殊的使用功能为目的制得的纤维,例如:负离子纤维中的负离子粉向环境中释放负离子,营造出仿大自然环境,给人以清新、舒适的感觉;远红外纤维具有吸收并反射远红外线的功能,促进人体的新陈代谢;抗红外线纤维则在军事中有着重要的作用;抗紫外线纤维则可阻挡日光中紫外线对人类皮肤的危害。
在这样的背景下,面对人们对纺织服装业提出新的要求,对于人们对美好生活的追求,如何让人们的穿着更加健康是纺织服装行业的奋斗目标之一,众所周知,日光中的紫外线以及衣物、家用纺织品中细菌的过度繁殖给人们带来一定的困扰,为此,不少研究者针对这些问题展开了研究,专利CN103114439A公开了一种具有生物调节作用的无纺布及其制备方法,该技术采用由含有益生菌的功能组合液配制成的整理剂处理,然后进行风干或者烘干而制成,然而该方法采用益生菌直接整理,容易造成益生菌失活,使得有效成分降低,持久性不足,功能单一,有待进一步改进。专利CN104783373A公开了一种防紫外线多色彩面料,包括下棉布层、羊毛层和上棉布层,但该面料制作复杂,采用染色纤维实现多彩目的,易产生污染,不符合当下绿色发展的时代特征。专利CN102071490A公开了一种有机光致变色纳米纤维,包括将有机光致变色化合物溶解在高分子溶液中,通过静电纺丝技术将该纺丝液制备成纳米纤维,通过变色来防紫外线,但是该纤维功能单一,而且存在光致变色现象不持久的问题,难以解决现有技术的问题。
因此,为了满足实际生活的需求,有必要提供一种含有益生菌微胶囊的功能性植物纤维,可兼具良好的抗菌性和防紫外线功效,来解决现有技术问题。
发明内容
针对现有技术中存在的问题,本发明的目的在于提供一种含有益生菌微胶囊的功能性植物纤维,所述含有益生菌微胶囊的功能性植物纤维可兼具良好的抗菌性和防紫外线功效,以较好地满足实际应用的需求。
为达此目的,本发明的技术方案如下:
本发明提供了一种含有益生菌微胶囊的功能性植物纤维,所述含有益生菌微胶囊的功能性植物纤维的制备方法包括以下步骤:
(1)将植物叶片原料清洗后粉碎成碎片状,然后与提取液体一起加入捏合机中,在温度为90-110℃、搅拌速度为100-200r/min的条件下提取4-6h,得到纺丝原液;
(2)将益生菌微胶囊加入到纺丝原液中,并充分搅拌均匀,然后湿法纺丝制成植物纤维;
(3)将增效剂加热至熔融状态,使用超声波雾化设备通过雾化的手段施加到植物纤维表面;
(4)然后再将植物纤维放入去离子水中浸渍,在30-45℃下脱水2-5min,随后在30-45℃条件下减压干燥,即制得功能性植物纤维。
在本发明含有益生菌微胶囊的功能性植物纤维的制备方法中,步骤(1)中,所述提取液体包括浓度为50-60%的N-甲基吗啉氧化物水溶液和没食子酸丙酯,所述N-甲基吗啉氧化物水溶液和没食子酸丙酯的质量比5-10:1。
在本发明含有益生菌微胶囊的功能性植物纤维的制备方法中,步骤(2)中,所述益生菌微胶囊的粒径为2-6μm,所述益生菌微胶囊的质量为植物叶片的1-1.2倍,所述益生菌微胶囊包括壳层和芯材,壳层为多巴胺,芯材为益生菌,所述壳层的厚度为0.7-1μm;所述湿法纺丝的凝固浴温度为40-50℃。
在本发明含有益生菌微胶囊的功能性植物纤维的制备方法中,步骤(3)中,所述增效剂的质量为植物纤维的0.5-0.6倍。
在本发明的一些实施方案中,所述益生菌微胶囊的制备方法包括以下步骤:
(1)在20-30℃下,将所得菌芯加入到4-羟乙基哌嗪丙磺酸缓冲溶液中,得到菌悬液,然后加入多巴胺,搅拌20-30min,使其混合均匀,形成混合液;
(2)将步骤(1)所得的液体放置在35-45℃的恒温下,将所述混合液的pH调节到8-9,使多巴胺自聚合,持续聚合1-2h,在菌芯的外周沉积形成聚多巴胺壳层后,产物即为益生菌微胶囊。
在本发明益生菌微胶囊的制备方法中,步骤(1)中,所述益生菌选自青春双歧杆菌或丁酸梭菌;所述混合液中,菌芯、多巴胺、4-羟乙基哌嗪丙磺酸缓冲溶液的质量比为:1:5-8:10-20,所述4-羟乙基哌嗪丙磺酸缓冲溶液的浓度为10-30mmol/L。
在本发明的一些实施方案中,所述增效剂的制备方法包括以下步骤:
(1)将碱式碳酸锌在450-480℃下煅烧5-10h,待冷却后进行研磨,然后与钛酸酯偶联剂JTW-131混合,经球磨、过筛,备用;将碳酸铈在500-600℃下煅烧5-10h,待冷却后进行研磨,然后加入氧化镧,混合均匀,烘干固体物,备用;
(2)将步骤(1)得到的备用物质与再生聚酯切片混合后,加入2,4-二羟基二苯甲酮,搅拌均匀,在90-110℃下干燥4-6h,经螺杆挤出机在200-220℃下熔融挤出、过水冷却、牵条、切粒和干燥,制成增效剂。
在本发明增效剂的制备方法中,所述碱式碳酸锌、碳酸铈与再生聚酯切片的质量比为1-2:1-2:1;步骤(1)中所述钛酸酯偶联剂JTW-131的质量为碱式碳酸锌的0.1-0.3倍,所述氧化镧的质量为碳酸铈的0.05-0.2倍;步骤(3)中所述2,4-二羟基二苯甲酮的质量为再生聚酯切片的0.05-0.1倍。
与现有技术相比,本发明具有以下有益效果:
(1)本发明采用微胶囊的方式,通过温和的条件,将益生菌包覆在多巴胺自聚合形成的外壳中,使用真空减压干燥方法,避免了高温对益生菌产生不良影响;其中,多巴胺在碱性的4-羟乙基哌嗪丙磺酸缓冲溶液中可快速自聚合,在菌芯外形成包覆层,具有耐酸、耐高温的性能,进一步保护益生菌,将该益生菌微胶囊在植物纤维中可以对金黄色葡萄球菌、大肠杆菌等有害病菌起到良好的抑制作用,同时,形成的多巴胺外壳,是天然黑色素中主要的色素之一,具有与黑色素相似的光吸收性能,在紫外光到可见光的范围内有宽波段的吸收,并且光吸收一直延伸至近红外区域,使制得的植物纤维具有防紫外线的效果。
(2)本发明所使用的增效剂,以碱式碳酸锌、碳酸铈和再生聚酯切片为原料,经一系列改性制备所得,并通过雾化的手段施加到植物纤维表面,一方面可以增强植物纤维的防紫外线效果,另一方面,在紫外光的照射下,能自行分解出带负电的电子,同时留下了带正电的空穴,这种空穴可以激发空气中的氧变为活性氧,与多种微生物发生氧化反应,从而把细菌杀死,尤其对金黄色葡萄球菌和大肠杆菌有良好的抑制作用。
其中,将碱式碳酸锌经煅烧、研磨后得到的产物属于N型半导体,当被紫外线照射时,价带上的电子能够吸收紫外线中的能量发生跃迁,将紫外线的能量变成分子的内能,从而达到抗紫外线的作用,再通过钛酸酯偶联剂JTW-131表面改性后,引入长链烷氧基,可改善纳米氧化锌与植物纤维的相容性,也能使植物纤维外观更好;将碳酸铈经煅烧、研磨后使用氧化镧进行改性,氧化镧能够增加紫外线的反射率和吸收率,减小紫外线的透过率,从而增强抗紫外线的作用,碳酸铈经煅烧、研磨后比表面积较大,具有一定的吸附作用,能够负载氧化镧,发挥出反射紫外线的功效;碱式碳酸锌、碳酸铈改性后与再生聚酯切片共同混熔融制得增效剂,该过程中使用2,4-二羟基二苯甲酮可以进一步保护纤维,使纤维长期受紫外线照射不会产生变质、老化,应用于功能性植物纤维的制备,可使制得的功能性植物纤维具有良好的抗紫外线性能和抗有害菌功能。
(3)本发明提供的含有益生菌微胶囊的功能性植物纤维,通过将益生菌微胶囊、增效剂加入植物纤维的制备,益生菌微胶囊与增效剂的协同使用,使得到的功能性植物纤维不仅具有良好的抑菌功能,还具有良好的防紫外线功能,在服装、家纺等纺织品中应用可以有效抑制衣服、地毯等纺织品中的病菌、虫螨,减少紫外线对人体的伤害。
具体实施方式
以下将结合具体实施方案来说明本发明。需要说明的是,下面的实施例为本发明的示例,仅用来说明本发明,而不用来限制本发明。在不偏离本发明主旨或范围的情况下,可进行本发明构思内的其他组合和各种改良。在以下实施例中,所使用到的化合物及相关试剂均可从市场购得,其中,碱式碳酸锌、碳酸铈购自兰州黄河锌镁纳米材料研究所,氧化镧购自赣州市广利高新技术材料有限公司,4-羟乙基哌嗪丙磺酸缓冲溶液购自武汉德晟生化科技有限公司,钛酸酯偶联剂JTW-131购自南京能德新材料技术有限公司,再生聚酯切片购自浙江海利环保科技股份有限公司。
实施例1
一种含有益生菌微胶囊的功能性植物纤维,所述含有益生菌微胶囊的功能性植物纤维的制备方法包括以下步骤:
(1)将100g菠萝叶片原料清洗后粉碎成碎片状,然后与150g提取液体一起加入捏合机中,在温度为110℃、搅拌速度为200r/min的条件下提取6h,得到纺丝原液;
(2)将120g益生菌微胶囊加入到纺丝原液中,并充分搅拌均匀,然后通过湿法纺丝制成菠萝纤维,凝固浴温度为40℃;
(3)取10g菠萝纤维,将6g增效剂加热至熔融状态,使用超声波雾化设备通过雾化的手段施加到菠萝纤维表面;
(4)然后再将菠萝纤维放入去离子水中浸渍,在45℃下脱水5min,随后在30℃条件下减压干燥,即制得功能性菠萝纤维。
其中,所述提取液体包括浓度为60%的N-甲基吗啉氧化物水溶液和没食子酸丙酯,所述N-甲基吗啉氧化物水溶液和没食子酸丙酯的质量比10:1,所述益生菌微胶囊的粒径为6μm,所述益生菌微胶囊包括壳层和芯材,壳层为多巴胺,芯材为益生菌,所述壳层的厚度为1μm。
其中,所述益生菌微胶囊的制备方法包括以下步骤:
(1)在30℃下,将所得100g青春双歧杆菌加入到1.5Kg浓度为30mmol/L的4-羟乙基哌嗪丙磺酸缓冲溶液中,得到菌悬液,然后加入800g多巴胺,搅拌30min,使其混合均匀,形成混合液;
(2)将步骤(1)所得的液体放置在35℃的恒温下,将所述混合液的pH调节到9,使多巴胺自聚合,持续聚合2h,在菌芯的外周沉积形成聚多巴胺壳层后,产物即为益生菌微胶囊。
其中,所述增效剂的制备方法包括以下步骤:
(1)将100g碱式碳酸锌在480℃下煅烧10h,待冷却后进行研磨,然后与30g钛酸酯偶联剂JTW-131混合,经球磨、过筛,备用;将100g碳酸铈在600℃下煅烧10h,待冷却后进行研磨,然后加入20g氧化镧,混合均匀,烘干固体物,备用;
(2)将步骤(1)得到的备用物质与100g再生聚酯切片混合后,加入10g2,4-二羟基二苯甲酮,搅拌均匀,在110℃下干燥6h,经螺杆挤出机在220℃下熔融挤出、过水冷却、牵条、切粒和干燥,制成增效剂。
实施例2
一种含有益生菌微胶囊的功能性植物纤维,所述含有益生菌微胶囊的功能性植物纤维的制备方法包括以下步骤:
(1)将100g菠萝叶片原料清洗后粉碎成碎片状,然后与150g提取液体一起加入捏合机中,在温度为90℃、搅拌速度为100r/min的条件下提取4h,得到纺丝原液;
(2)将100g益生菌微胶囊加入到纺丝原液中,并充分搅拌均匀,然后通过湿法纺丝制成菠萝纤维,凝固浴温度为40℃;
(3)取10g菠萝纤维,将5g增效剂加热至熔融状态,使用超声波雾化设备通过雾化的手段施加到菠萝纤维表面;
(4)然后再将菠萝纤维放入去离子水中浸渍,在30℃下脱水2min,随后在30℃条件下减压干燥,即制得功能性菠萝纤维。
其中,所述提取液体包括浓度为50%的N-甲基吗啉氧化物水溶液和没食子酸丙酯,所述N-甲基吗啉氧化物水溶液和没食子酸丙酯的质量比5∶1,所述益生菌微胶囊的粒径为2μm,所述益生菌微胶囊包括壳层和芯材,壳层为多巴胺,芯材为益生菌,所述壳层的厚度为0.7μm。
其中,所述益生菌微胶囊的制备方法包括以下步骤:
(1)在20℃下,将所得100g青春双歧杆菌加入到1.2Kg浓度为30mmol/L的4-羟乙基哌嗪丙磺酸缓冲溶液中,得到菌悬液,然后加入500g多巴胺,搅拌20min,使其混合均匀,形成混合液;
(2)将步骤(1)所得的液体放置在45℃的恒温下,将所述混合液的pH调节到8,使多巴胺自聚合,持续聚合1h,在菌芯的外周沉积形成聚多巴胺壳层后,产物即为益生菌微胶囊。
其中,所述增效剂的制备方法包括以下步骤:
(1)将100g碱式碳酸锌在450℃下煅烧5h,待冷却后进行研磨,然后与30g钛酸酯偶联剂JTW-131混合,经球磨、过筛,备用;将100g碳酸铈在500℃下煅烧5h,待冷却后进行研磨,然后加入20g氧化镧,混合均匀,烘干固体物,备用;
(2)将步骤(1)得到的备用物质与100g再生聚酯切片混合后,加入10g2,4-二羟基二苯甲酮,搅拌均匀,在110℃下干燥6h,经螺杆挤出机在220℃下熔融挤出、过水冷却、牵条、切粒和干燥,制成增效剂。
实施例3
一种含有益生菌微胶囊的功能性植物纤维,所述含有益生菌微胶囊的功能性植物纤维的制备方法包括以下步骤:
(1)将100g菠萝叶片原料清洗后粉碎成碎片状,然后与150g提取液体一起加入捏合机中,在温度为90℃、搅拌速度为100r/min的条件下提取4h,得到纺丝原液;
(2)将110g益生菌微胶囊加入到纺丝原液中,并充分搅拌均匀,然后通过湿法纺丝制成菠萝纤维,凝固浴温度为40℃;
(3)取10g菠萝纤维,将5.5g增效剂加热至熔融状态,使用超声波雾化设备通过雾化的手段施加到菠萝纤维表面;
(4)然后再将菠萝纤维放入去离子水中浸渍,在40℃下脱水3.5min,随后在30℃条件下减压干燥,即制得功能性菠萝纤维。
其中,所述提取液体包括浓度为50%的N-甲基吗啉氧化物水溶液和没食子酸丙酯,所述N-甲基吗啉氧化物水溶液和没食子酸丙酯的质量比8∶1,所述益生菌微胶囊的粒径为5μm,所述益生菌微胶囊包括壳层和芯材,壳层为多巴胺,芯材为益生菌,所述壳层的厚度为0.85μm。
其中,所述益生菌微胶囊的制备方法包括以下步骤:
(1)在20℃下,将所得100g青春双歧杆菌加入到1.2Kg浓度为30mmol/L的4-羟乙基哌嗪丙磺酸缓冲溶液中,得到菌悬液,然后加入650g多巴胺,搅拌20min,使其混合均匀,形成混合液;
(2)将步骤(1)所得的液体放置在45℃的恒温下,将所述混合液的pH调节到8,使多巴胺自聚合,持续聚合1h,在菌芯的外周沉积形成聚多巴胺壳层后,产物即为益生菌微胶囊。
其中,所述增效剂的制备方法包括以下步骤:
(1)将100g碱式碳酸锌在450℃下煅烧5h,待冷却后进行研磨,然后与20g钛酸酯偶联剂JTW-131混合,经球磨、过筛,备用;将100g碳酸铈在500℃下煅烧5h,待冷却后进行研磨,然后加入10g氧化镧,混合均匀,烘干固体物,备用;
(2)将步骤(1)得到的备用物质与100g再生聚酯切片混合后,加入5g2,4-二羟基二苯甲酮,搅拌均匀,在90℃下干燥6h,经螺杆挤出机在200℃下熔融挤出、过水冷却、牵条、切粒和干燥,制成增效剂。
实施例4
与实施例1的区别在于:在增效剂的制备中,碱式碳酸锌、碳酸铈与再生聚酯切片的质量比为5:1:0.5。
实施例5
与实施例1的区别在于:在功能性植物纤维的制备中,所使用的益生菌微胶囊的质量为植物叶片的0.5倍。
实施例6
与实施例1的区别在于:在功能性植物纤维的制备中,所使用的益生菌微胶囊的质量为植物叶片的0.1倍。
对比例1
与实施例1的区别在于:不添加益生菌微胶囊。
对比例2
与实施例1的区别在于:不添加增效剂。
对比例3
与实施例1的区别在于:在增效剂的制备中不使用碱式碳酸锌。
对比例4
与实施例1的区别在于:在增效剂的制备中不使用氧化铈。
将各实施例、对比例制备的功能性植物纤维进行性能测试,断裂强度、断裂伸长率测试方法参照GB/T9997-1988进行,纤维抑菌率测试参照GB/T20944.3—2008《纺织品抗菌性能的评价第3部分:振荡法》进行,纤维的抗紫外线效果按GB/T18830-2009测试紫外线透过率,具体情况见表1。
表1实施例、对比例制备的功能性植物纤维性能测试结果
由对比例1、实施例5与实施例1的测试结果比较可知,在功能性植物纤维的制备中使用特定用量的益生菌微胶囊可有效提高金黄色葡萄球菌、大肠杆菌的抑制率;对比例2、对比例3、对比例4、实施例4、实施例6与实施例1比较可知,在功能性植物纤维的制备中使用特定比例的增效剂,可有效降低紫外线透过率。综合比较各实施例、对比例的测试结果可知,本发明提供的功能性植物纤维,不仅具有良好的抗菌性,还具有优异的防紫外线功能,具有良好的应用前景。
以上实施方式只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人了解本发明内容并加以实施,并不能以此限制本发明的保护范围,凡根据本发明精神实质所做的等效变化或修饰,都应涵盖在本发明的保护范围内。
Claims (10)
1.一种含有益生菌微胶囊的功能性植物纤维,其特征在于,由包含如下制备步骤的制备方法制备得到:
(1)将植物叶片原料清洗后粉碎成碎片状,然后与提取液体一起加入捏合机中,在温度为90-110℃、搅拌速度为100-200r/min的条件下提取4-6h,得到纺丝原液;
(2)将益生菌微胶囊加入到纺丝原液中,并充分搅拌均匀,然后通过湿法纺丝制成植物纤维;
(3)将增效剂加热至熔融状态,使用超声波雾化设备通过雾化的手段施加到植物纤维表面;
(4)然后再将植物纤维放入去离子水中浸渍,在30-45℃下脱水2-5min,随后在30-45℃条件下减压干燥,即制得功能性植物纤维。
2.根据权利要求1所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,步骤(1)中所述的提取液体包括浓度为50-60%的N-甲基吗啉氧化物水溶液和没食子酸丙酯,所述N-甲基吗啉氧化物水溶液和没食子酸丙酯的质量比5-10∶1。
3.根据权利要求1所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,步骤(2)中所述益生菌微胶囊的粒径为2-6μm,所述益生菌微胶囊的质量为植物叶片的1-1.2倍;所述益生菌微胶囊包括壳层和芯材,壳层为多巴胺,芯材为益生菌,所述壳层的厚度为0.7-1μm,所述湿法纺丝的凝固浴温度为40-50℃。
4.根据权利要求1所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,步骤(3)中所述增效剂的质量为植物纤维的0.5-0.6倍。
5.根据权利要求1所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,所述益生菌微胶囊的制备方法包括以下步骤:
(1)在20-30℃下,将所得菌芯加入到4-羟乙基哌嗪丙磺酸缓冲溶液中,得到菌悬液,然后加入多巴胺,搅拌20-30min,使其混合均匀,形成混合液;
(2)将步骤(1)所得的液体放置在35-45℃的恒温下,将所述混合液的pH调节到8-9,使多巴胺自聚合,持续聚合1-2h,在菌芯的外周沉积形成聚多巴胺壳层后,产物即为益生菌微胶囊。
6.根据权利要求5所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,步骤(1)中所述益生菌选自青春双歧杆菌或丁酸梭菌;所述混合液中菌芯、多巴胺、4-羟乙基哌嗪丙磺酸缓冲溶液的质量比为:1:5-8:10-20,4-羟乙基哌嗪丙磺酸缓冲溶液的浓度为10-30mmol/L。
7.根据权利要求1所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,所述增效剂的制备方法包括以下步骤:
(1)将碱式碳酸锌在450-480℃下煅烧5-10h,待冷却后进行研磨,然后与钛酸酯偶联剂JTW-131混合,经球磨、过筛,备用;将碳酸铈在500-600℃下煅烧5-10h,待冷却后进行研磨,然后加入氧化镧,混合均匀,烘干固体物,备用;
(2)将步骤(1)得到的备用物质与再生聚酯切片混合,加入2,4-二羟基二苯甲酮,搅拌均匀,在90-110℃下干燥4-6h,经螺杆挤出机在200-220℃下熔融挤出、过水冷却、牵条、切粒和干燥,制成增效剂。
8.根据权利要求7所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,所述碱式碳酸锌、碳酸铈与再生聚酯切片的质量比为1-2:1-2:1。
9.根据权利要求7所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,步骤(1)中所述钛酸酯偶联剂 JTW-131的质量为碱式碳酸锌的0.1-0.3倍;所述氧化镧的质量为碳酸铈的0.05-0.2倍。
10.根据权利要求7所述的含有益生菌微胶囊的功能性植物纤维,其特征在于,步骤(3)中所述2,4-二羟基二苯甲酮的质量为再生聚酯切片的0.05-0.1倍。
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