CN114774593A - 一种去除糖汁中色素的方法 - Google Patents
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Abstract
本发明公开了一种去除糖汁中色素的方法,通过膜滤蔗汁与氨基功能化自浮微球混合吸附蔗汁中的色素。所述的氨基功能化自浮微球是以中空玻璃微球表面在经过高温强碱刻蚀后作为吸附剂载体,利用多巴胺天然界面“胶水”特性,聚乙烯亚胺和盐酸多巴胺在刻蚀中空玻璃微球表面共接枝制备而成,通过引入氨基官能团,对膜滤蔗汁中吸附质(带负电色素)具有优异的靶向吸附性能。所制备的吸附剂具有自浮性能,无需额外能耗和设备就可以实现微球与膜滤蔗汁自主分离;通过本方法与膜法绿色制糖工艺耦合,解决膜分离技术处理甘蔗汁无法截留其中小分子色素导致成品白砂糖色值偏高的技术问题,实现制糖全过程绿色化。
Description
技术领域
本发明涉及一种去除糖汁中色素的方法,属于制糖工程技术领域。
背景技术
蔗糖是生活必需品,也是重要的工业原料,目前甘蔗食糖生产中,绝大部分制糖企业仍是沿用传统亚硫酸法来生产耕地白砂糖,其主要包含压榨、清净、蒸发及结晶四个工序。在蔗汁清净过程,需加入较大数量化学助剂提纯蔗汁,如CaO、SO2、H3PO4及PAM等,不仅增加了食糖加工成本,且残留在成品糖中的化学助剂成分(尤其是SO2及合成PAM残留单体)还将成为食糖安全的隐患。全面推行绿色制造是实现制造强国目标的重要任务之一,大力发展绿色加工技术是解决传统制造业发展中资源与能源瓶颈问题的关键,要加大技术改造力度、加快产业重组及“二次创业”。
陶瓷膜分离技术是一种高效、环保的物理分离提纯技术,已在食品、医药、化工、发酵等众多领域广泛应用。基于陶瓷膜分离技术在众多领域的出色表现,使得人们相信它具有引发未来糖业革命的潜能。本专利发明人对陶瓷膜应用于蔗汁体系的过滤澄清进行了较为详尽的研究,发现甘蔗汁经孔径为5~50nm的陶瓷膜过滤后,不仅可以去除(截留)蔗汁中近100%的悬浮杂质及部分大分子色素,还可以获得较大的膜渗透通量以满足工业化生产的需求。但陶瓷膜过滤较难截留一些分子量较小的色素,而甘蔗汁中的小分子色素在煮糖结晶时极易被包裹在蔗糖晶体的内部,导致膜法砂糖色值偏高。因此,对膜滤蔗汁小分子色素的去除,已成了膜法甘蔗绿色制糖的技术瓶颈。
发明内容
本发明的目的是提供一种去除糖汁中色素的方法,解决膜法绿色制糖过程,采用膜分离技术过滤甘蔗汁,无法截留甘蔗汁中的小分子色素,导致成品白砂糖色值偏高的技术问题。
为实现上述目的,本发明采用了以下的技术手段:
一种去除糖汁中色素的方法,将糖汁经陶瓷膜过滤后,与氨基功能化自浮微球充分搅拌得到糖汁氨基功能化自浮微球混合液,将糖汁氨基功能化自浮微球混合液静置后进行固液分离,获得脱色糖汁。
所述的氨基功能化自浮微球通过以下方法制备:
(1)将中空玻璃微球、浓度为1%~3%的盐酸溶液按质量体积比为1.0~1.5g:20~50mL的比例混合均匀,搅拌反应2h;
(2)将洗净中空玻璃微球及浓度为0.5~1.5mol/L的氢氧化钠溶液按质量体积比为2.0~6.0g:25~100mL的比例混合均匀,升高至80℃后,300~700r/min的转速搅拌,搅拌反应8h,得到刻蚀微球;
(3)盐酸多巴胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为0.5~2.0g:50~200mL的比例混合均匀,得到碱性多巴胺溶液;
(4)聚乙烯亚胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为1.5~6.0g:50~200mL的比例混合均匀,得到聚乙烯亚胺溶液;
(5)刻蚀微球、碱性多巴胺溶液与聚乙烯亚胺溶液按质量体积比为0.5~3.0g:50~300mL:50~300mL的比例混合均匀,搅拌12~24h;
(6)氨基功能化自浮微球微球依次采用无水乙醇及蒸馏水交替洗涤3次,在50℃下真空干燥至恒重。
所述的Tris-HCL缓冲液pH值为8.5。
所述的糖汁氨基功能化自浮微球混合液中糖汁与氨基功能化自浮微球按以下比例混合:糖汁:氨基功能化自浮微球为200~500mL:1.0g。
所述的陶瓷膜的孔径为5~50nm。
所述的将糖汁氨基功能化自浮微球混合液静置的时间为:10min。
所述的搅拌是在磁力搅拌器中进行。
与现有技术比较,本发明具有的有益效果:
(1)中空玻璃微球(HGM)具有成本低、重量轻、化学稳定性好、无毒等特点,是制备自浮吸附剂理想基材,易实现吸附剂回收及再利用。本发明以中空玻璃微球为原料制备糖用脱色剂,在引入吸附氨基官能团聚乙烯亚胺(PEI)作用下,改性氨基HGM对膜滤糖汁中吸附质(带负电色素)具有优异的靶向吸附性能,且保持中空及密闭性,还易回收易再生。
(2)将氨基功能化自浮微球与膜法绿色制糖工艺耦合,既保留了膜分离技术处理甘蔗汁优越的澄清除杂优势,又克服了膜过滤无法脱除甘蔗汁中小分子色素导致成品糖色值高的缺陷,相比于现有的亚硫酸法制糖,推动制糖全过程绿色化。
(3)在现有技术中,糖汁脱色剂主要分为生物质活性炭及以苯乙烯与二乙烯基苯为基体合成的阴离子交换树脂。活性炭没有交换性能,不能去离子型色素,且吸附产生的消耗量大,固废多,难再生。而苯乙烯及二乙烯基苯均来源于石油,其原料不可再生,且它们均被国际癌症研究机构列为2B类致癌物。显然,将此类树脂用于食糖纯化,会存在食品安全隐患。此外,活性炭与树脂在吸附过程中固液分离能耗大,成本高。本发明以中空玻璃微球为原料制备糖用脱色剂来吸附去除膜滤蔗汁剩余色素,具有原料获取方便、价格便宜、稳定无毒等优势。
(4)本发明将以均匀规律定性结构中空玻璃微球作为基材制备的吸附剂,相比于现有的无定型吸附剂比表面积更大,可提供更多的吸附位点,使吸附剂易于和蔗汁中的色素充分接触并发生吸附反应实现脱色。
(5)现有的吸附剂(如活性炭等)通常为无定型吸附剂,当发生吸附反应结束后,需要采用板框压滤机将吸附剂和吸附质进行分离。而本发明制备的吸附剂具有自浮性能,当其吸附蔗汁中色素结束后,可快速自主固液分离,具有设备结构紧凑、分离效率高、出产能力大、无需附属设备等优点。
附图说明
图1为本发明所述的氨基功能化自浮微球微球的扫描电子显微镜微观图。
图2为本发明所述的氨基功能化自浮微球微球吸附清汁后的扫描电子显微镜微观图。
图3为膜滤蔗汁经微球吸附剂处理前后的色值。
具体实施方式
下面结合附图及实施例对本发明进行进一步的描述。
中空玻璃微球来源规格型号:购买于中钢马鞍山新材料科技有限公司,产品型号为GS40。糖汁来源于广西百桂堂食品科技有限公司。
实施例1
一种去除糖汁中色素的方法,包括如下步骤:
(1)经孔径为5nm陶瓷膜过滤后的糖汁,与氨基功能化自浮微球微球按体积质量比为200mL:1.0g的比例,在膜滤清汁箱中充分混合均匀,反应0.5h;
(2)静置10min,吸附色素后的氨基功能化自浮微球与蔗汁自主分离,得到脱色糖汁;
(3)脱色糖汁经蒸发浓缩及煮糖结晶后,得到白砂糖;
(4)将吸附色素后的氨基功能化自浮微球依次采用0.5mol/L碳酸氢钠及0.1mol/L的氢氧化钠溶液浸泡2h后,用蒸馏水将其洗涤至中性,循环使用。
所述的氨基功能化自浮微球的制备,包括如下步骤:
(1)将中空玻璃微球、浓度为1%的盐酸溶液按质量体积比为1.0g:50mL的比例混合均匀,搅拌反应2h,去除杂质及灰尘;
(2)将洗净中空玻璃微球及浓度为0.5mol/L氢氧化钠溶液按质量体积比为2g:100mL的比例混合均匀,升高至80℃后,300r/min的转速搅拌,从而获得均一溶液,搅拌反应8h,得到刻蚀微球;
(3)盐酸多巴胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为0.5g:200mL的比例混合均匀,得到碱性多巴胺溶液;
(4)聚乙烯亚胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为1.5g:200mL的比例混合均匀,得到聚乙烯亚胺溶液;
(5)刻蚀微球碱性、多巴胺溶液与聚乙烯亚胺溶液按质量体积比为0.5g:300mL:300mL的比例混合均匀,搅拌12h,利用多巴在弱碱性条件下的自聚和聚多巴/聚乙烯亚胺共聚物的粘附能力,将聚多巴/聚乙烯亚胺涂层包裹在刻蚀微球表面,自浮分离;
(6)氨基功能化自浮微球微球依次采用无水乙醇及蒸馏水交替洗涤3次,在50℃下真空干燥至恒重。
在氨基功能化自浮微球的制备方法中,所述的Tris-HCL缓冲液,其pH值为8.5,步骤(1)、(2)及(5)所述的搅拌均使用磁力搅拌器进行搅拌。
实施例1中,制备出的自浮微球吸附前后如附图1、2所示。所制备的自浮微球表面为多空网络结构,在吸附色素后,孔隙被色素填满,表面变得平滑。
实施例1中,膜滤清汁经氨基功能化自浮微球吸附处理前后,其中的蔗糖分并无显著差异,表明微球吸附剂不会吸附蔗汁中的蔗糖分子;而膜滤清汁经氨基功能化自浮微球吸附处理前后,其色值如附图3所示,从图3可以看出,膜滤清汁经微球吸附剂处理后,可大幅度降低其色值。
实施例2
一种去除糖汁中色素的方法,包括如下步骤:
(1)经孔径为8nm陶瓷膜过滤后的甘蔗混合汁与氨基功能化自浮微球微球按体积质量比为300mL:1.0g的比例,在膜滤清汁箱中充分混合均匀,反应1h;
(2)静置10min,吸附色素后的氨基功能化自浮微球与蔗汁自主分离,得到脱色糖汁;
(3)脱色糖汁经蒸发浓缩及煮糖结晶后,得到白砂糖;
(4)将吸附色素后的氨基功能化自浮微球依次采用0.5mol/L碳酸氢钠及1.0mol/L的氢氧化钠溶液浸泡2h后,用蒸馏水将其洗涤至中性,循环使用。
在膜滤蔗汁的脱色方法中,步骤(1)所述的氨基功能化自浮微球的制备方法,包括如下步骤:
(1)将中空玻璃微球、浓度为2%的盐酸溶液按质量体积比为1.2g:40mL的比例混合均匀,搅拌反应2h,去除杂质及灰尘;
(2)将洗净中空玻璃微球及浓度为1.0mol/L的氢氧化钠溶液按质量体积比为3g:50mL的比例混合均匀,升高至80℃后,600r/min的转速搅拌,从而获得均一溶液,搅拌反应8h,得到刻蚀微球;
(3)盐酸多巴胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为1.0g:100mL的比例混合均匀,得到碱性多巴胺溶液;
(4)聚乙烯亚胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为3.0g:100mL的比例混合均匀,得到聚乙烯亚胺溶液;
(5)刻蚀微球碱性、多巴胺溶液与聚乙烯亚胺溶液按质量体积比为2.0g:100mL:100mL的比例混合均匀,搅拌18h,利用多巴在弱碱性条件下的自聚和聚多巴/聚乙烯亚胺共聚物的粘附能力,将聚多巴/聚乙烯亚胺涂层包裹在刻蚀微球表面,自浮分离;
(6)氨基功能化自浮微球微球依次采用无水乙醇及蒸馏水交替洗涤3次,在50℃下真空干燥至恒重。
在氨基功能化自浮微球的制备方法中,所述的Tris-HCL缓冲液,其pH值为8.5,步骤(1)、(2)及(5)所述的搅拌均使用磁力搅拌器进行搅拌。
膜滤清汁经氨基功能化自浮微球吸附处理前后,其色值如附图3所示,从图3可以看出,膜滤清汁经微球吸附剂处理后,可大幅度降低其色值。
实施例3
一种去除糖汁中色素的方法,包括如下步骤:
(1)经孔径为50nm陶瓷膜过滤后的甘蔗混合汁与氨基功能化自浮微球微球按体积质量比为500mL:1.0g的比例,在膜滤清汁箱中充分混合均匀,反应2h;
(2)静置10min,吸附色素后的氨基功能化自浮微球与蔗汁自主分离,得到脱色糖汁;
(3)脱色糖汁经蒸发浓缩及煮糖结晶后,得到白砂糖;
(4)将吸附色素后的氨基功能化自浮微球依次采用0.5mol/L碳酸氢钠及1.0mol/L的氢氧化钠溶液浸泡2h后,用蒸馏水将其洗涤至中性,循环使用。
在膜滤蔗汁的脱色方法中,步骤(1)所述的氨基功能化自浮微球的制备方法,包括如下步骤:
(1)将中空玻璃微球、浓度为3%的盐酸溶液按质量体积比为1.5g:20mL的比例混合均匀,搅拌反应2h,去除杂质及灰尘;
(2)将洗净中空玻璃微球及浓度为1.5mol/L的氢氧化钠溶液按质量体积比为6.0g:25mL的比例混合均匀,升高至80℃后,700r/min的转速搅拌,从而获得均一溶液,搅拌反应8h,得到刻蚀微球;
(3)盐酸多巴胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为2.0g:50mL的比例混合均匀,得到碱性多巴胺溶液;
(4)聚乙烯亚胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为6.0g:50mL的比例混合均匀,得到聚乙烯亚胺溶液;
(5)刻蚀微球碱性、多巴胺溶液与聚乙烯亚胺溶液按质量体积比为3.0g:50mL:50mL的比例混合均匀,搅拌24h,利用多巴在弱碱性条件下的自聚和聚多巴/聚乙烯亚胺共聚物的粘附能力,将聚多巴/聚乙烯亚胺涂层包裹在刻蚀微球表面,自浮分离;
(6)氨基功能化自浮微球微球依次采用无水乙醇及蒸馏水交替洗涤3次,在50℃下真空干燥至恒重。
在氨基功能化自浮微球的制备方法中,所述的Tris-HCL缓冲液,其pH值为8.5,步骤(1)、(2)及(5)所述的搅拌均使用磁力搅拌器进行搅拌。
膜滤清汁经氨基功能化自浮微球吸附处理前后,其色值如附图3所示,从图3可以看出,膜滤清汁经微球吸附剂处理后,可大幅度降低其色值。
Claims (7)
1.一种去除糖汁中色素的方法,其特征在于,将糖汁经陶瓷膜过滤后,与氨基功能化自浮微球充分搅拌得到糖汁氨基功能化自浮微球混合液,将糖汁氨基功能化自浮微球混合液静置后进行固液分离,获得脱色糖汁。
2.根据权利要求1所述的除糖汁中色素的方法,其特征在于,所述的氨基功能化自浮微球通过以下方法制备:
(1)将中空玻璃微球、浓度为1%~3%的盐酸溶液按质量体积比为1.0~1.5g:20~50mL的比例混合均匀,搅拌反应2h;
(2)将洗净中空玻璃微球及浓度为0.5~1.5mol/L的氢氧化钠溶液按质量体积比为2.0~6.0g:25~100mL的比例混合均匀,升高至80℃后,300~700r/min的转速搅拌,搅拌反应8h,得到刻蚀微球;
(3)盐酸多巴胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为0.5~2.0g:50~200mL的比例混合均匀,得到碱性多巴胺溶液;
(4)聚乙烯亚胺与浓度为50mmol/L Tris-HCL缓冲液按质量体积比为1.5~6.0g:50~200mL的比例混合均匀,得到聚乙烯亚胺溶液;
(5)刻蚀微球、碱性多巴胺溶液与聚乙烯亚胺溶液按质量体积比为0.5~3.0g:50~
300mL:50~300mL的比例混合均匀,搅拌12~24h;
(6)氨基功能化自浮微球微球依次采用无水乙醇及蒸馏水交替洗涤3次,在50℃下
真空干燥至恒重。
3.根据权利要求2所述的除糖汁中色素的方法,其特征在于,所述的Tris-HCL缓冲液pH值为8.5。
4.根据权利要求1所述的除糖汁中色素的方法,其特征在于,所述的糖汁氨基功能化自浮微球混合液中糖汁与氨基功能化自浮微球按以下比例混合:糖汁:氨基功能化自浮微球为200~500mL:1.0g。
5.根据权利要求1所述的除糖汁中色素的方法,其特征在于,所述的陶瓷膜的孔径为5~
50nm。
6.根据权利要求1所述的除糖汁中色素的方法,其特征在于,所述的将糖汁氨基功能化自浮微球混合液静置的时间为:10min。
7.根据权利要求1所述的除糖汁中色素的方法,其特征在于,所述的搅拌是在磁力搅拌器中进行。
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