CN106046722B - 全生物降解仿生鱼饵及其制备方法 - Google Patents
全生物降解仿生鱼饵及其制备方法 Download PDFInfo
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- CN106046722B CN106046722B CN201610396168.8A CN201610396168A CN106046722B CN 106046722 B CN106046722 B CN 106046722B CN 201610396168 A CN201610396168 A CN 201610396168A CN 106046722 B CN106046722 B CN 106046722B
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- fish bait
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- bionic fish
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Abstract
本发明涉及一种全生物降解仿生鱼饵及其制备方法，属于高分子材料领域。由包含以下重量份的组分制成：聚乳酸99‑80份，增韧剂1‑20份，活化剂0.01‑10份，催化剂0.05‑2份，成核剂0.1‑5份，诱食剂0.01‑5份，颜料0‑3份，抗氧剂0‑1份，润滑剂0‑1份。将混合均匀的物料加入到双螺杆挤出机料斗中，控制增韧剂注入量与聚乳酸的重量比为1:99‑20:80，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒；得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。所述的双螺杆挤出机挤出温度为140‑190℃，螺杆长径比L/D=44:1‑64:1，螺杆转速为80rpm‑360rpm；所述的注塑机注塑温度为130‑200℃，注塑压力50‑120MPa，保压时间5s‑300s，模具温度为60‑120℃。
Description
技术领域
本发明涉及一种高分子材料的制备领域，具体地说是一种全生物降解仿生鱼饵及其制备方法。
背景技术
众所周知，随着人们经济水平的提高，垂钓作为一项户外活动深受现代人们的喜爱。垂钓用塑料制备的仿生鱼饵具有逼真的仿生鱼、虾、虫等效果，同时可长期使用，无需换饵等特点，在垂钓爱好者中被广泛使用。然而常用塑料仿生鱼饵多是用不可降解的塑料制备而成，如采用PVC、PE、PC、ABS等塑料。这类塑料制备的仿生鱼饵一旦脱落掉入海洋，上百年都无法降解，会对海洋生物及生态环境造成极大的危害。
聚乳酸（PLA）是由植物中提取淀粉、经发酵成乳酸、进一步聚合而成的生物降解高分子材料，聚乳酸具有优异的成型加工性能。用聚乳酸材料制备的仿生鱼饵脱落掉入海洋中时，可以在自然界的微生物作用下完全降解为H2O和CO2，不会对海洋生态环境带来任何危害。但聚乳酸材料脆性大、不耐热（55℃即发生变形），不经改性不利于成型加工。
专利CN104497509A提供了一种可以降解的仿生鱼饵，由聚乳酸材料制成，为了提高聚乳酸材料的韧性，同时材料中还添加有聚己内酯和TPEE热塑性弹性体。该方法生产的仿生鱼饵一方面会因添加有聚己内酯这种生物降解材料而使生产成本增加，另一方面会因添加有TPEE热塑性弹性体而破坏了聚乳酸的全生物降解特性。
发明内容
为了克服现有技术的不足，本发明提供一种全生物降解仿生鱼饵及其制备方法，有很好的韧性和耐热性能，同时本发明提供的仿生鱼饵不仅可以完全生物降解，不会对环境带来任何危害，而且还具有很好的诱食效果，可提高鱼类的捕食率。
本发明解决其技术问题所采用的技术方案是：一种全生物降解仿生鱼饵及其制备方法，其特征在于，由包含以下重量份的组分制成：
聚乳酸 99-80份，
增韧剂 1-20份，
活化剂 0.01-10份，
催化剂 0.05-2份，
成核剂 0.1-5份，
诱食剂 0.01-5份，
颜料 0-3份，
抗氧剂 0-1份，
润滑剂 0-1份。
所述的聚乳酸由L-乳酸、D-乳酸、或DL-乳酸中的一种或一种以上聚合得到。
所述的增韧剂为分子链中含有羟基、或羧基的化合物。
所述的活化剂是分子链中含有2个或2个以上环氧基官能团的化合物。
所述的催化剂为二水合氯化亚锡、辛酸亚锡、四丁基锡、三氧化二锑、三氧化二铝、氧化锌中的一种或一种以上。
所述的成核剂为有机成核剂、无机成核剂中的一种或一种以上；其中有机成核剂为酰肼类化合物、酰胺类化合物、取代芳基磷酸金属盐类化合物、苯基磷酸锌中的一种或一种以上；无机成核剂为滑石粉、纳米蒙脱土、纳米碳酸钙、气相白炭黑中的一种或一种以上。
所述的诱食剂为氨基酸、硫代甜菜碱、大蒜素、牛磺酸、乙基麦芽酚、乳酸乙酯、香兰素、香豆素、中草药粉中的一种或一种以上。
所述的抗氧剂为受阻酚类、亚磷酸酯类、含硫抗氧剂中的一种或一种以上。
所述的润滑剂为硬脂酸及其盐类、酰胺类、石蜡、聚乙烯蜡、油酸中的一种或一种以上。
一种制备所述全生物降解仿生鱼饵的方法，其特征在于所包括如下步骤：
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸99-80份、活化剂0.01-10份、催化剂0.05-2份、成核剂0.1-5份、诱食剂0.01-5份、颜料0-3份、抗氧剂0-1份、润滑剂0-1份于高混机中混合均匀；
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂注入量与聚乳酸的重量比为1:99-20:80，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒；
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵；
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=44:1-64:1，螺杆转速为80rpm-360rpm；
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力50-120MPa，保压时间5s-300s，模具温度为60-120℃。
本发明的有益效果是，选用合适的增韧剂、活化剂和成核剂，并配合高长径比的双螺杆挤出机，使原料在挤出机中充分混合，并且充分实现原位聚合反应，一方面可以获得所需的聚乳酸大分子链结构，另一方面使成核剂在共混物体系中分散均匀，再结合相应的注塑工艺，使得制备的仿生鱼饵具有很好的韧性和耐热性能；同时本发明提供的仿生鱼饵不仅可以完全生物降解，不会对环境带来任何危害，而且还具有很好的诱食效果，可提高鱼类的捕食率。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例1：
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸（浙江海正公司生产，牌号REVODE201）99份、活化剂甲基丙烯酸缩水甘油酯0.01份、催化剂二水合氯化亚锡0.05份、成核剂癸二酸二苯甲酰肼1份、诱食剂牛磺酸0.01份、颜料铁红0.5份、抗氧剂1010 0.3份、抗氧剂168 0.1份于高混机中混合均匀。
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂聚蓖麻油注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂聚蓖麻油的注入量与聚乳酸的重量比为1:99，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒。
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=44:1，螺杆转速为80rpm。
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力50MPa，保压时间5s，模具温度为60℃。
本方法中选用的增韧剂韧性优越、活化剂分子链上的环氧基官能团活性高。一方面增韧剂分子链上的羟基或羧基与活化剂分子链上的环氧基官能团反应，另一方面聚乳酸分子链端的羟基或羧基也会与活化剂分子链上的环氧基官能团反应，这样就将增韧剂分子链通过活化剂分子链接到聚乳酸分子链上，提高了聚乳酸的韧性。同时，本方法中选用的增韧剂分子链中含有多个羟基或羧基官能团，在活化剂分子的作用下与聚乳酸分子反应可以形成多支链结构、或是网状结构的大分子链，这种大分子链相互之间易发生缠结；与此同时，本方法中配合选择合适的结晶成核剂，来提高聚乳酸材料的结晶度，利用聚乳酸大分子链之间的相互缠结和提高结晶度两种方式相结合，提高了聚乳酸材料的耐热性。
实施例2：
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸（深圳光华伟业公司生产，牌号注塑级）90份、活化剂ADR4370S 0.5份、催化剂辛酸亚锡0.2份、成核剂十二烷二酸二苯甲酰肼0.1份、成核剂滑石粉(6000目)1份、诱食剂鱼腥草粉0.3份、诱食剂香豆素0.05份、颜料酞菁1份、抗氧剂1076 0.5份、抗氧剂626 0.5份、润滑剂硬脂酸钙0.3份于高混机中混合均匀。
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂蓖麻油注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂蓖麻油的注入量与聚乳酸的重量比为10:90，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒。
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=52:1，螺杆转速为200rpm。
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力80MPa，保压时间60s，模具温度为90℃。
实施例3
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸（美国NatureWorks公司生产，牌号3051D）85份、活化剂环氧大豆油10份、催化剂三氧化二锑2份、成核剂乙撑双硬脂酰胺0.1份、诱食剂硫代甜菜碱1份、诱食剂小茴香粉0.5份、颜料钴蓝0.3份、抗氧剂DLTDP 0.2份、抗氧剂618 0.2份、润滑剂硬脂酸0.2份于高混机中混合均匀。
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂棕榈油注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂棕榈油的注入量与聚乳酸的重量比为15:85，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒。
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=60:1，螺杆转速为250rpm。
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力100MPa，保压时间300s，模具温度为120℃。
实施例4
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸（美国NatureWorks公司生产，牌号3052D）88份、活化剂ADR4368 3份、催化剂氧化锌1份、成核剂取代芳基磷酸锂盐0.8份、成核剂纳米蒙脱土1.2份、诱食剂L-脯氨酸1份、诱食剂阿魏粉4份、颜料钛白粉3份、抗氧剂2246 0.3份、抗氧剂TNP 0.2份、润滑剂芥酸酰胺0.3份于高混机中混合均匀。
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂亚麻籽油注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂亚麻籽油的注入量与聚乳酸的重量比为12:88，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒。
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=64:1，螺杆转速为360rpm。
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力120MPa，保压时间30s，模具温度为110℃。
实施例5
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸（美国NatureWorks公司生产，牌号3001D）92份、活化剂ADR4300 0.2份、催化剂四丁基锡0.3份、成核剂纳米碳酸钙4份、成核剂苯基磷酸锌1份、诱食剂乳酸乙酯0.2份、诱食剂桂皮粉0.2份、颜料群青0.2份、抗氧剂BHT0.2份、抗氧剂300 0.1份、润滑剂聚乙烯蜡1份于高混机中混合均匀。
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂聚蓖麻油注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂聚蓖麻油的注入量与聚乳酸的重量比为8:92，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒。
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=60:1，螺杆转速为280rpm。
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力90MPa，保压时间28s，模具温度为110℃。
实施例6
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸（美国NatureWorks公司生产，牌号6202D）80份、活化剂ADR4370S 0.5份、催化剂三氧化二铝0.8份、成核剂TMC-328 0.6份、成核剂气相白炭黑0.2份、诱食剂乙基麦芽酚0.3份、诱食剂灵草粉0.1、润滑剂石蜡1份份于高混机中混合均匀。
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂蓖麻油注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂蓖麻油的注入量与聚乳酸的重量比为20:80，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒。
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵。
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=56:1，螺杆转速为260rpm。
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力95MPa，保压时间20s，模具温度为110℃。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
所述的增韧剂优选蓖麻油、聚蓖麻油、亚麻籽油、棕榈油中的一种或一种以上。
所述的活化剂是分子链中含有2个或2个以上环氧基官能团的化合物，优选环氧大豆油、甲基丙烯酸缩水甘油酯、巴斯夫公司生产的ADR-4370S、ADR-4368、ADR-4300中的一种或一种以上。
所述的催化剂二水合氯化亚锡、辛酸亚锡、四丁基锡、三氧化二锑、三氧化二铝、氧化锌中的一种或一种以上。
所述的成核剂为有机成核剂、无机成核剂中的一种或一种以上；有机成核剂优选酰肼类化合物、酰胺类化合物、取代芳基磷酸金属盐类化合物、苯基磷酸锌中的一种或一种以上；无机成核剂优选滑石粉、纳米蒙脱土、纳米碳酸钙、气相白炭黑、中的一种或一种以上。
所述酰肼类化合物优选癸二酸二苯甲酰肼、壬二酸二苯甲酰肼、辛二酸二苯甲酰肼、十二烷二酸二苯甲酰肼、十三烷二酸二苯甲酰肼中的一种或一种以上；所述酰胺类化合物优选油酸酰胺、芥酸酰胺、乙撑双硬脂酰胺、商品名为TMC-328中的一种或一种以上；所述的取代芳基磷酸金属盐类化合物优选取代芳基磷酸锂盐、取代芳基磷酸铝盐中的一种或一种以上。
所述的诱食剂为氨基酸、硫代甜菜碱、大蒜素、牛磺酸、乙基麦芽酚、乳酸乙酯、香兰素、香豆素、中草药粉中的一种或一种以上。所述的中草药粉进一步优选麝香粉、阿魏粉、甘草粉、桂皮粉、八角粉、丁香粉、香松粉、排草粉、灵草粉、鱼腥草粉、墨旱莲粉、小茴香粉、沉香粉、川芎粉中的一种或一种以上。
所述的颜料为有机颜料、无机颜料中的一种或一种以上，有机颜料优选偶氮颜料、酞菁颜料、喹吖啶酮颜料，无机颜料优选炭黑、钛白粉、铁红、铅铬黄、锌铬黄、镉黄、铁黄、氧化铬绿、铅铬绿、铁蓝、钴蓝、群青、铁棕。
所述的抗氧剂为受阻酚类、亚磷酸酯类、含硫抗氧剂中的一种或一种以上；所述的受阻酚类抗氧剂优选2,6-二叔丁基对甲酚(抗氧剂BHT)、2,2'-硫代双(4-甲基-6-叔丁基苯酚)(抗氧剂2246)、四[β-（3,5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯（抗氧剂1010）、β-（3,5-二叔丁基-4-羟基苯基）丙酸十八碳醇酸酯（抗氧剂1076）中的一种或一种以上；所述的亚磷酸酯类抗氧剂优选三（2.4-二叔丁基苯基）亚磷酸酯（抗氧剂168）、双（2,4 一二叔丁基苯基）季戊四醇二磷酸酯(抗氧剂626)、双（十八烷基）季戊四醇二亚磷酸酯(抗氧剂618)、三(壬基苯基)亚磷酸酯(抗氧剂TNP)中的一种或一种以上；所述的含硫抗氧剂优选硫代二丙酸双十二醇酯(抗氧剂DLTDP)、硫代二丙酸双十八烷酯(抗氧剂DSTDP)、4-4’-硫代双酚类抗氧剂(抗氧剂300)、2,2’-硫代双[3-(3,5-二叔丁基-4-羟基苯基)丙酸乙酯](抗氧剂1035)中的一种或一种以上。
所述的润滑剂为硬脂酸及其盐类、酰胺类、石蜡、聚乙烯蜡、油酸中的一种或一种以上。
在上述全生物降解仿生鱼饵材料组分中，还可以根据需要添加本技术领域常用的填料，如碳酸钙、滑石粉、二氧化硅、云母、木粉、秸秆粉、谷物壳粉、蒙脱土、黏土等。
Claims (6)
1.一种全生物降解仿生鱼饵，其特征在于，其原料包含以下重量份的组分：
聚乳酸 99-80份，
增韧剂 1-20份，
活化剂 0.01-10份，
催化剂 0.05-2份，
成核剂 0.1-5份，
诱食剂 0.01-5份，
颜料 0-3份，
抗氧剂 0-1份，
润滑剂 0-1份；
所述的增韧剂为分子链中含有羟基、或羧基的化合物；
所述的活化剂是分子链中含有2个或2个以上环氧基官能团的化合物；
所述的催化剂为二水合氯化亚锡、辛酸亚锡、四丁基锡、三氧化二锑、三氧化二铝、氧化锌中的一种或一种以上；
所述的成核剂为有机成核剂、无机成核剂中的一种或一种以上；其中有机成核剂为酰肼类化合物、酰胺类化合物、取代芳基磷酸金属盐类化合物、苯基磷酸锌中的一种或一种以上；无机成核剂为滑石粉、纳米蒙脱土、纳米碳酸钙、气相白炭黑中的一种或一种以上。
2.根据权利要求1所述全生物降解仿生鱼饵，其特征在于所述的聚乳酸由L-乳酸、D-乳酸、或DL-乳酸中的一种或一种以上聚合得到。
3.根据权利要求1所述全生物降解仿生鱼饵，其特征在于所述的诱食剂为氨基酸、硫代甜菜碱、大蒜素、牛磺酸、乙基麦芽酚、乳酸乙酯、香兰素、香豆素、中草药粉中的一种或一种以上。
4.根据权利要求1所述全生物降解仿生鱼饵，其特征在于所述的抗氧剂为受阻酚类、亚磷酸酯类、含硫抗氧剂中的一种或一种以上。
5.根据权利要求1所述全生物降解仿生鱼饵，其特征在于所述的润滑剂为硬脂酸及其盐类、酰胺类、石蜡、聚乙烯蜡、油酸中的一种或一种以上。
6.一种制备权利要求1所述全生物降解仿生鱼饵的方法，其特征在于所包括如下步骤：
(1)将聚乳酸树脂干燥后，按重量份数称取聚乳酸99-80份、活化剂0.01-10份、催化剂0.05-2份、成核剂0.1-5份、诱食剂0.01-5份、颜料0-3份、抗氧剂0-1份、润滑剂0-1份于高混机中混合均匀；
(2)将步骤(1)混合均匀的物料加入到双螺杆挤出机料斗中，开启双螺杆挤出机主机和主喂料开关，同时通过双螺杆挤出机的液体进料口采用液体计量泵将增韧剂注入到双螺杆挤出机中，调节双螺杆挤出机主喂料转速和液体计量泵的流量，控制增韧剂注入量与聚乳酸的重量比为1:99-20:80，进行熔融挤出、拉条、冷却、切粒并干燥，得到改性聚乳酸颗粒；
(3)将步骤(2)得到的改性聚乳酸颗粒在注塑机上注塑成型，得到所需形状的全生物降解仿生鱼饵；
步骤(2)中所述的双螺杆挤出机挤出温度为140-190℃，螺杆长径比L/D=44:1-64:1，螺杆转速为80rpm-360rpm；
步骤(3)中所述的注塑机注塑温度为130-200℃，注塑压力50-120MPa，保压时间5s-300s，模具温度为60-120℃。
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| EP3698644A1 (en) * | 2019-02-20 | 2020-08-26 | Kl-Teho Oy | A fishing bait, a mouldable composition for manufacturing the fishing bait, a method for manufacturing the fishing bait and a use of the mouldable composition |
| CN110343374A (zh) * | 2019-07-10 | 2019-10-18 | 安徽宏飞钓具有限公司 | 一种环保可降解的仿生鱼饵 |
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