CN114075351A - 一种可食性海藻吸管及其制备方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明提供一种以海藻酸钠为主要原料制备的一种可食性海藻吸管,是将粘度为10‑100MPa·s的海藻酸钠和田菁胶、柔软剂制成凝胶溶液,凝胶溶液中均匀涂布在模具上,并进行烘干;烘干的模具浸没于二价金属盐的食用酸溶液中,浸泡后通过后续的常规吸管步骤制成可食性海藻吸管。本发明制备的可食性海藻吸管是一种可食性生物材料,具有安全、无塑化剂、无毒副作用,100%全生物降解,耐酸及耐超高温和低温等特点。制备的可食性海藻吸管的拉伸强度在70‑100MPa之间,断裂伸长率在5‑8%之间,水溶性小于3%。本发明的海藻吸管具有热稳定性,强力学性能和阻隔性能,是塑料吸管的有效代替品,具有明显的使用价值和潜在的消费市场。
Description
技术领域
本发明属于吸管技术领域,具体涉及一种可食性海藻吸管及其制备方法。
技术背景
塑料污染是世界性难题,地球上平均每一天用掉约50亿支塑料吸管,随着社会的发展,塑料吸管的大量使用导致塑化剂问题也越来越突出,塑料吸管中的塑化剂,会随着饮品温度的提高,加速释放进入体内,形成致癌物质,若长期食用可引起生殖系统异常、甚至造成畸及癌症,而难以被降解的塑料吸管,又会对生态环境造成极大的破坏和污染,威胁人类的身体健康。“塑化剂”问题也越来越突出,世界各国政府及地方政府相继发布禁塑令,并且都在加大力度支持寻求替代品,然而,在日常生活中,人们仍对吸管类产品表现出大量需求,随着各国及各级政府限塑令等条款的制约,塑料吸管将陆续退出市场。
可食性海藻吸管是采用了海藻酸钠为主要原料,通过海藻酸钠与食用钙锌交联形成凝胶后,其均匀的截面形貌及热稳定性,增强了海藻吸管的力学性能和阻隔性能,并且海藻吸管具有可食性和全生物降解性,可以克服塑料吸管导致塑化剂对人体的各种危害,具有较高的使用价值。
发明内容
本发明的目的是提供一种以海藻酸钠为主要原料制备的一种可食性海藻吸管,吸管具有安全、生物降解率高、耐酸性、具有温度耐受性等特点。本发明所提供的海藻吸管是塑料吸管有效代替品,同时具有较高的使用价值和巨大的消费市场。
本发明的可食性海藻吸管,是用如下方法制备的:
1)将特定粘度的海藻酸钠和田菁胶、柔软剂制成凝胶溶液,真空脱气,脱气后的凝胶溶液粘度保持在6000-20000Pa·s范围内;
所述的海藻酸钠的粘度为10-100MPa·s,其中优选20-50MPa·s。
所述的田菁胶,全部或部分用量使用其它食品用胶来替代;
所述的食品胶为卡拉胶、阿拉伯胶、罗望子多糖胶、琼脂、果胶、黄原胶、β-环状糊精或羟丙甲基纤维素。
所述的柔软剂,优选为藻酸丙二醇酯,其在胶液中的质量百分比浓度为0.05-2.0%
所述的田菁胶在胶溶液中的添加量质量体积百分比浓度为0.1-10.0%;
所述的海藻酸钠在胶溶液中的添加量质量百分比浓度为0.5-10.0%;
所述的真空脱气时,保持溶液的温度为40-60℃;
2)在制备吸管的模具上涂防黏连物,然后将1)中制备的凝胶溶液中均匀涂布在模具上,并进行烘干;
作为实施例的一种具体记载,所述的制备吸管的模具,为不锈钢模条;
所述的防黏连物,一个实施例的具体记载为食用油;所述的食用油优选植物油脂,包括菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油、葡萄籽油、核桃油及牡丹籽油。
所述的烘干,作为一个实施例的具体记载,是在30-100℃条件下烘干;
3)将2)中烘干的模具浸没于二价金属盐的食用酸溶液中,浸泡后通过后续的常规吸管步骤制成可食性海藻吸管。
上述的二价金属盐包括食用钙盐和食用锌盐,优选乳酸钙。
所述的食用酸为柠檬酸,醋酸或乳酸;
所述的3)中的后续常规步骤,为清洗,烘干,脱模,修整步骤。
本发明制备的可食性海藻吸管是一种可食性生物材料,具有安全、无塑化剂、无毒副作用,100%全生物降解,耐酸(pH1-7)及耐超高温和低温(-80℃-120℃)等特点。制备的可食性海藻吸管的拉伸强度在70-100MPa之间,断裂伸长率在5-8%之间,水溶性小于3%,6-12个月内可被土壤微生物全部降解。本发明的海藻吸管具有热稳定性,强力学性能和阻隔性能,是塑料吸管的有效代替品,具有明显的使用价值和潜在的消费市场。
附图说明
图1:海藻酸钠粘度26MPa·s,浓度9.%,田菁胶浓度0.0%的混合膜扫描电镜2000倍的表面图(左)和5000倍横截面图(右);
图2:海藻酸钠粘度26MPa·s,浓度9.%,田菁胶浓度1.0%的混合膜扫描电镜2000倍的表面图(左)和5000倍横截面图(右);
图3:海藻酸钠粘度26MPa·s,浓度8.0.%,田菁胶浓度2.0%的混合膜扫描电镜2000倍的表面图(左)和5000倍横截面图(右);
图4:海藻酸钠粘度26MPa·s,浓度7.0%,田菁胶浓度3.0%的混合膜扫描电镜2000倍的表面图(左)和5000倍横截面(右);
图5:海藻酸钠粘度26MPa·s,浓度6.0%,田菁胶浓度4.0%的混合膜扫描电镜2000倍的表面图(左)和5000倍横截面(右);
图6:海藻酸钠浓度0.0%,田菁胶浓度10.0%的混合膜扫描电镜2000倍的表面图(左)和5000倍横截面(右);
图7:不同添加比例海藻酸钠/田菁胶协同作用傅里叶红外光谱图。
具体实施方式
本发明所提供的可食性海藻吸管,是将海藻酸钠和食品用胶(优选为田菁胶)相混合,再浸入二价金属盐的食用酸溶液中进行交联,在改善了海藻酸钠成膜皱缩性的同时,又极大提高了海藻酸钙膜的抗拉伸强度,并且还增加了断裂伸长率,使海藻吸管既有强度又有韧性。通过傅里叶变换红外光谱分析了海藻酸钠膜、海藻酸钠/田菁胶复合膜以及田菁胶膜的组成和不同组分之间的相互作用。如图7所示,海藻酸钠膜于3323、1600、1418、1085和1030cm-1处有特征峰。其中,3323cm-1处的特征峰是由-OH的伸缩震动引起的,1600cm-1和1418cm-1处的特征峰分别对应-COOH的反对称和对称伸缩振动吸收峰,1030cm-1处为糖苷键吸收峰。田菁胶膜在官能团区和指纹区产生了较多的特征峰,在1400cm-1处特征峰的峰面积大于其他膜,除此之外特征峰无其他膜尖锐,但随着田菁胶质量比的增加,羟基处的特征峰往高波长方向发生明显的偏移,这主要的由于田菁胶中含有大量的邻位顺式羟基,有规则的半乳糖支链形成与海藻酸钠结合,使得电子云密度平均化,红外光谱图进一步说明田菁胶与海藻酸钠发生了很大程度上的反应,二者有很好的融合。扫描电镜是最直观有效的观察到膜结构和相容性的方法,可直接观察混合膜的自由表面,从而分析薄膜的混合及分布情况。如图1-图6所示,不同浓度的田菁胶对海藻酸钠膜的皱缩性有极大的改善,海藻酸钠膜和复合膜表面光滑,无明显的颗粒,膜的横截面未出现裂纹或孔隙,有条理规则的结构,可见其致密性良好,没有出现明显的相分离,有良好的相容性。
本发明的可食性海藻吸管,其一种制备方法是首先称取定量的特定粘度的海藻酸钠和田菁胶按一定比例混合,加入藻酸丙二醇酯柔软剂,搅拌,再加入蒸馏水,在40℃-60℃的水温中持续搅拌至形成透明均一溶液,然后保温真空脱气,直至溶液中无气泡产生,脱气的热溶液粘度在40-60℃范围内保持在6000-20000Pa·s范围内。再取一定长度和直径的实心不锈钢模条,在其表面用少量的食用油,然后将模条插入脱气后的热的混合胶液中蘸胶,拔出模条上下左右旋转,直到胶液均匀涂布在不锈钢模条上,在30-100℃条件下烘干,然后将蘸胶的模条浸没于一定浓度的金属盐酸溶液中,浸泡2-30分钟后,拔出用蒸馏水冲洗,烘干,脱模,修整,即可得到本发明的可食性海藻吸管。
所述的海藻酸钠特定粘度10-100MPa·s之间(MPa.s为毫帕斯卡·秒),此粘度大小代表海藻酸钠的分子量的大小,采用旋转式粘度计测定。因为如果海藻酸钠粘度小于10MPas,水溶液中海藻酸钠含量可以达到10%左右,但是由于海藻酸钠的分子量太小,所得海藻吸管的强度也太小,容易断裂,机械性能太差;如果海藻酸钠粘度大于100MPas,由于粘度太大,水溶液中海藻酸钠含量最高只能达到2%左右,由于褐藻酸钠含量较低,最后所得海藻吸管壁太薄,吸管太软,强度不够;优选海藻酸钠粘度为20-50MPa·s,这种情况下水溶液中海藻酸钠含量可以达到3.0-9.0%之间,田菁胶浓度在0.1-10.0%之间,最后所得海藻吸管不论是拉伸强度和断裂伸长率,都能达到吸管的要求。
所使用的田菁胶可改变了海藻酸钠膜的化学组成和分子间的相互作用力,二者之间有较强的协同作用,添加量控制在0.1-10.0%之间,拉伸强度达到70-100MPa之间,断裂伸长率达到5-8%之间,无论硬度还是韧性,都适合做海藻吸管。如果海藻酸钠与其他食品胶结合,可能会得到拉伸强度超过100MPa,硬度很大,但是这种情况下,断裂伸长率都会低于5%,这样所得海藻吸管太硬太脆,韧性不够,同样容易断裂,同样如果海藻酸钠与其他食品胶结合可能会得到断裂伸长率超过8%,甚至达到15%左右,韧性很好,但是拉伸强度一般在40-60MPa之间,硬度不够,优选田菁胶。也可再添加田菁胶的基础上,再添加其他食品胶如:卡拉胶,阿拉伯胶,罗望子多糖胶,琼脂,果胶,黄原胶,β-环状糊精,羟丙甲基纤维素。
所述的脱气的热溶液粘度保持在6000-20000Pa·s范围内,粘度代表溶液的粘稠度,采用旋转式粘度计测定。由于海藻酸钠的含量比较高,所以混合液的热粘度(40-60℃)也高,一旦冷却,混合液会变成半固体状态,没有流动性,不锈钢模条就无法蘸胶,脱气后的热溶液具有较好的流动性,粘度在6000-20000Pa·s之间溶液流动性较好,容易蘸胶,才能保证所得海藻吸管的厚度,硬度,韧性更加合理。
所述的食用油优选植物油脂,包括菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油、葡萄籽油、核桃油及牡丹籽油。
所述的二价金属盐和食用酸溶液,二价金属盐包括钙盐和锌盐。因为吸管是食品专用材料,对人体有益的金属离子而且又可以与海藻酸钠形成强凝胶的主要是钙离子和锌离子,优选乳酸钙;食用酸包括柠檬酸,醋酸,乳酸,优选柠檬酸。
所述的藻酸丙二醇酯,是一种在酸性条件下非常稳定的柔软剂,pH在1-5的范围内非常稳定。
本发明的可食性海藻吸管能够达到100%全生物降解,在pH值1-7和-80-120℃之间是稳定的,所以在冷饮和热饮的情况下,海藻吸管不会发生变形,而且水溶性小于3%,可有效替代塑料吸管,解决塑化剂对人体的危害。
吸管膜机械性能的测定方法如下:
根据ASTM Method D882方法,将样品切割成5cm×1.5cm的条状,使用TMS-Pro质构仪进行测试。主要测试参数为:设定初始夹距30mm,拉伸速度60mm/min。
拉伸强度(TS)和断裂伸长率(EB)计算公式如下:
TS=Fmax/A
其中,Fmax表示样品膜断裂所需要的最大力(N);A表示样品膜的横截面积(样品膜厚度×样品膜宽,m2)。
EB=L/L0×100%
其中,L表示样品膜断裂时的伸长量(m);L0表示样品膜起始夹距的长(m)。
下面结合具体实施例对本发明的可食性海藻吸管及其制备方法进行详细描述。
实施例1
首先称取26MPa·s粘度的海藻酸钠8.0g,田菁胶2.0g,藻酸丙二醇酯0.1g,搅拌,加入100ml蒸馏水,在40℃-60℃的水温中持续搅拌至形成透明均一溶液,然后保温真空脱气,直至溶液中无气泡产生,脱气的热溶液粘度8000MPa·s范围内。用长200mm直径7mm的实心不锈钢模条,在其表面用少量食用油涂抹,然后将模条插入脱气后的热的混合胶液中蘸胶,拔出模条上下左右旋转,直到胶液均匀涂布在不锈钢模条上,在60℃条件下烘干,然后将蘸胶的模条浸没于2%浓度的乳酸钙和0.5%的柠檬酸的混合溶液中,浸泡8分钟后,取出用蒸馏水冲洗,然后将不锈钢模条膜在50℃烘干,脱模,修整,即可得到本发明的可食性海藻吸管。
海藻吸管的拉伸强度79MPa,断裂伸长率达到7.66%,水溶性小于2.38%,6-12个月内可被土壤微生物全部降解。
实施例2
首先称取50MPa·s粘度的海藻酸钠6.0g,田菁胶4.0g,藻酸丙二醇酯0.15克,搅拌,加入100ml蒸馏水,在40℃-60℃的水温中持续搅拌至形成透明均一溶液,然后保温真空脱气,直至溶液中无气泡产生,脱气的热溶液粘度12000MPa·s范围内。用长200mm直径7mm的实心不锈钢模条,在其表面用少量食用油涂抹,然后将模条插入脱气后的热的混合胶液中蘸胶,拔出模条上下左右旋转,直到胶液均匀涂布在不锈钢模条上,在60℃条件下烘干,然后将蘸胶的模条浸没于2%浓度的乳酸钙和0.5%的柠檬酸的混合溶液中,浸泡10分钟后,取出用蒸馏水冲洗,然后将不锈钢模条膜在50℃烘干,脱模,修整。
即可得到本发明的可食性海藻吸管。海藻吸管的拉伸强度76MPa,断裂伸长率达到7.78%,水溶性小于2.67%,6-12个月内可被土壤微生物全部降解。
实施例3
首先称取83MPa·s粘度的海藻酸钠3.5g,田菁胶1.5g,藻酸丙二醇酯0.15克,卡拉胶0.1克,搅拌,加入100ml蒸馏水,在40℃-60℃的水温中持续搅拌至形成透明均一溶液,然后保温真空脱气,直至溶液中无气泡产生,脱气的热溶液粘度15600MPa·s范围内。用长200mm直径7mm的实心不锈钢模条,在其表面用少量食用油涂抹,然后将模条插入脱气后的热的混合胶液中蘸胶,拔出模条上下左右旋转,直到胶液均匀涂布在不锈钢模条上,在60℃条件下烘干,然后将蘸胶的模条浸没于2%浓度的乳酸钙和0.5%的柠檬酸的混合溶液中,浸泡10分钟后,取出用蒸馏水冲洗,然后将不锈钢模条膜在50℃烘干,脱模,修整。
即可得到本发明的可食性海藻吸管。海藻吸管的拉伸强度73MPa,断裂伸长率达到7.82%,水溶性小于2.49%,6-12个月内可被土壤微生物全部降解。
实施例4
首先称取20MPa·s粘度的海藻酸钠9.0g,田菁胶1.0g,藻酸丙二醇酯0.15克,羟丙甲基纤维素0.1克,搅拌,加入100ml蒸馏水,在40℃-60℃的水温中持续搅拌至形成透明均一溶液,然后保温真空脱气,直至溶液中无气泡产生,脱气的热溶液粘度14400MPa·s范围内。用长200mm直径7mm的实心不锈钢模条,在其表面用少量食用油涂抹,然后将模条插入脱气后的热的混合胶液中蘸胶,拔出模条上下左右旋转,直到胶液均匀涂布在不锈钢模条上,在60℃条件下烘干,然后将蘸胶的模条浸没于2%浓度的乳酸钙和0.5%的柠檬酸的混合溶液中,浸泡10分钟后,取出用蒸馏水冲洗,然后将不锈钢模条膜在50℃烘干,脱模,修整。
即可得到本发明的可食性海藻吸管。海藻吸管的拉伸强度86MPa,断裂伸长率达到7.84%,水溶性小于2.72%,6-12个月内可被土壤微生物全部降解。
实施例5
首先称取20MPa·s粘度的海藻酸钠9.0g,田菁胶0.0g,藻酸丙二醇酯0.15克,羟丙甲基纤维素0.1克,搅拌,加入100ml蒸馏水,在40℃-60℃的水温中持续搅拌至形成透明均一溶液,然后保温真空脱气,直至溶液中无气泡产生,脱气的热溶液粘度9200MPa·s范围内。用长200mm直径7mm的实心不锈钢模条,在其表面用少量食用油涂抹,然后将模条插入脱气后的热的混合胶液中蘸胶,拔出模条上下左右旋转,直到胶液均匀涂布在不锈钢模条上,在60℃条件下烘干,然后将蘸胶的模条浸没于2%浓度的乳酸钙和0.5%的柠檬酸的混合溶液中,浸泡10分钟后,取出用蒸馏水冲洗,然后将不锈钢模条膜在50℃烘干,脱模,修整。
本实施例得到的可食性海藻吸管的拉伸强度46MPa,断裂伸长率达到4.87%,拉伸强度小于70MPa,断裂伸长率小于5.0,吸管脆且易断裂;表明不添加田菁胶制备的吸管满足不了使用要求。
Claims (16)
1.一种可食性海藻吸管,其特征在于,所述的可食性海藻吸管使用如下的方法制备的:
1)将特定粘度的海藻酸钠和田菁胶、柔软剂制成凝胶溶液,真空脱气,脱气后的凝胶溶液粘度保持在6000-20000Pa·s范围内;
2)在制备吸管的模具上涂布防黏连物,然后将1)中制备的凝胶溶液涂布在模具上,并进行烘干;
3)将2)中烘干的模具浸于二价金属盐的食用酸溶液中,浸泡后通过后续的常规吸管步骤制成可食性海藻吸管。
2.如权利要求1所述的可食性海藻吸管,其特征在于,所述的1)中海藻酸钠的粘度为10—100MPa·s。
3.如权利要求1所述的可食性海藻吸管,其特征在于,所述的1)中海藻酸钠的粘度为20—50MPa·s。
4.如权利要求1所述的可食性海藻吸管,其特征在于,所述的1)中田菁胶,全部或部分用量使用其它食品用胶来替代。
5.如权利要求4所述的可食性海藻吸管,其特征在于,所述的食品胶为卡拉胶、阿拉伯胶、罗望子多糖胶、琼脂、果胶、黄原胶、β-环状糊精或羟丙甲基纤维素。
6.如权利要求1所述的可食性海藻吸管,其特征在于,所述的柔软剂为藻酸丙二醇酯。
7.如权利要求6所述的可食性海藻吸管,其特征在于,所述的柔软剂藻酸丙二醇酯在凝胶溶液中的质量百分比浓度为0.05-2.0%。
8.如权利要求1所述的可食性海藻吸管,其特征在于,所述的1)中田菁胶在凝胶溶液中的添加量质量体积百分比浓度为0.1-10.0%。
9.如权利要求1所述的可食性海藻吸管,其特征在于,所述的1)中海藻酸钠在胶溶液中的添加量质量百分比浓度为0.5-10.0%。
10.如权利要求1所述的可食性海藻吸管,其特征在于,所述的1)中的真空脱气时保持溶液的温度为40-60℃。
11.如权利要求1所述的可食性海藻吸管,其特征在于,所述的2)中的防黏连物为食用油。
12.如权利要求11所述的可食性海藻吸管,其特征在于,所述的食用油包括菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油、葡萄籽油、核桃油或牡丹籽油。
13.如权利要求1所述的可食性海藻吸管,其特征在于,所述的3)中的二价金属盐包括食用钙盐和食用锌盐。
14.如权利要求13所述的可食性海藻吸管,其特征在于,所述的二价金属盐为乳酸钙。
15.如权利要求1所述的可食性海藻吸管,其特征在于,所述的3)中所述的食用酸为柠檬酸,醋酸或乳酸。
16.如权利要求1所述的可食性海藻吸管,其特征在于,所述的3)中所述的的后续常规步骤,为清洗,烘干,脱模,修整步骤。
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