CN101921342B - 一种交联辛烯基琥珀酸木薯淀粉酯的制备方法 - Google Patents

一种交联辛烯基琥珀酸木薯淀粉酯的制备方法 Download PDF

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CN101921342B
CN101921342B CN2010102869367A CN201010286936A CN101921342B CN 101921342 B CN101921342 B CN 101921342B CN 2010102869367 A CN2010102869367 A CN 2010102869367A CN 201010286936 A CN201010286936 A CN 201010286936A CN 101921342 B CN101921342 B CN 101921342B
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tapioca starch
octenyl succinate
starch sodium
crosslinked
sodium octenyl
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CN101921342A (zh
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金征宇
李彬
谢正军
王金鹏
田耀旗
徐学明
杨哪
夏洁人
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Jiangnan University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/9258Velocity
    • B29C2948/9259Angular velocity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885Screw or gear
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

一种交联辛烯基琥珀酸木薯淀粉酯的制备方法,属于食品技术领域。本发明以木薯淀粉作为原料,以三偏磷酸钠为交联剂,以辛烯基琥珀酸酐为酯化剂,经过双螺杆挤压机挤压后,再经干燥、冷却、粉碎而制得。本法制得的产品交联辛烯基琥珀酸木薯淀粉酯取代度范围为0.011-1.020,沉降体积范围为0.5-2.5mL,在国内首次用挤压法生产了交联辛烯基琥珀酸木薯淀粉酯,并且为交联辛烯基琥珀酸木薯淀粉酯在食品工业中的应用提供了基础。

Description

一种交联辛烯基琥珀酸木薯淀粉酯的制备方法
技术领域
一种交联辛烯基琥珀酸木薯淀粉酯的制备方法,属于食品技术领域。
背景技术
辛烯基琥珀酸淀粉酯有较大的分子量,在油水界面处可形成一层强度很大的薄膜,可以稳定水包油型的乳浊液。它还有稳定性和增稠性及增加乳液的光泽度的功能,在水包油型的乳液中有着特殊的作用,可用于不同粘度的各种乳化液。辛烯基琥珀酸淀粉酯还有优良的自由流动性和斥水性,能防止淀粉料粒的附聚,在水的乳液中能均匀分散,稳定规定的淀粉含量和所需粘度的乳化液,并且有好的流动性。将其经过交联变性后,其黏度增高,抗剪切力强,耐酸碱性好。由于它所特有的性能和功能,因而它可广泛用于各类食品中。
采用双螺杆挤压技术生产交联辛烯基琥珀酸木薯淀粉酯,酯化和交联反应同时完成,使工艺大为简便,无污水产生,使生产成本降低。挤压法生产交联辛烯基琥珀酸木薯淀粉酯,淀粉的糊化同时发生可以改善湿法生产出的产品使用前要经过蒸煮后才能溶解在水中的缺点。
本发明为实现采用双螺杆挤压技术大规模生产交联辛烯基琥珀酸木薯淀粉酯奠定了很好的基础。
发明内容
本发明的目的是提供一种交联辛烯基琥珀酸木薯淀粉酯的制备方法。
本发明的技术方案:一种交联辛烯基琥珀酸木薯淀粉酯的制备方法,以木薯淀粉作为原料,以三偏磷酸钠为交联剂,以辛烯基琥珀酸酐为酯化剂,经过双螺杆挤压机挤压,同时完成酯化和交联反应后,再经冷却、干燥、粉碎而制得;
物料质量配比为木薯淀粉100份,交联剂0.8-2份,酯化剂0.8-1.5份,氢氧化钠0.08-0.1份;
工艺为:按配比称取木薯淀粉,加入交联剂三偏磷酸钠,氢氧化钠,和用辛烯基琥珀酸酐5倍质量乙醇溶解的辛烯基琥珀酸酐溶液,然后放在30-40℃烘箱内将乙醇烘去,加蒸馏水调节水分含量至30%,混合均匀;将所述物料密封,在40-50℃条件下保温1-2小时;调节挤压条件,螺杆转速70-150r/min,挤压机三段温度分别设定为50-60℃,80-90℃,100-130℃;将所述物料放入挤压机内挤压,同时完成交联与酯化反应;反应后在30-40℃对挤出物进行干燥,在室温下冷却,粉碎,置于密封样品袋包装。
沉降体积的检测:准确称取0.5克绝干的交联辛烯基琥珀酸木薯淀粉酯样品于100mL烧杯中,准确加入25mL蒸馏水,配制成质量分数为2%的溶液。将烧杯置于82-85℃的水浴中,稍加搅拌,保温2min,取出冷却至室温。取两支刻度离心管,分别加入上述得到的糊液10mL,对称放入离心机内,启动离心机,缓慢加速至4000r/min,离心2min。取出离心管,将上层清液倒入另一支同样体积的离心管中,读出毫升数,计算沉降体积。对同一样品进行2次平行测定,取平均值。
沉降体积(mL)=10-V(mL),V为上清液的体积。
取代度(DS)的测定:称取1.5克交联辛烯基琥珀酸木薯淀粉酯样品置于100mL烧杯中,加入50mL 95%乙醇,在磁力搅拌器搅拌10min,加入15mL 2.5mol/L盐酸的乙醇溶液酸化30min。将酸化后样品倒入布式漏斗,用90%乙醇抽滤洗涤至无Cl-离子(用硝酸银检验)。将洗涤后的样品烘干,称量后移入250mL三角瓶并加入100mL蒸馏水,沸水浴20min,加2滴酚酞,趁热用0.1mol/LNaOH滴定至粉红色。取代度DS计算公式如下:
DS=0.1624A/(1-0.210A)             式(1)
A=CV/W                          式(2)
式(1)中:A-每克交联辛烯基琥珀酸木薯淀粉酯所耗用0.1mol/LNaOH标准溶液的物质的量,mmol/g;0.1624-葡萄糖残基的摩尔质量,g/mol;0.210-辛烯基琥珀酸酐的摩尔质量,g/mol;式(2)中:C-NaOH标准溶液的摩尔浓度,mol/L;V-样品滴定所耗用NaOH标准溶液的体积,mL;W-样品的质量,g。
本发明的有益效果:本发明采用双螺杆挤压技术生产交联辛烯基琥珀酸木薯淀粉酯,酯化和交联反应同时完成,使工艺大为简便,无污水产生,使生产成本降低。挤压法生产交联辛烯基琥珀酸木薯淀粉酯,淀粉的糊化同时发生可以改善湿法生产出的产品使用前要经过蒸煮后才能溶解在水中的缺点。
本法制得的产品交联辛烯基琥珀酸木薯淀粉酯取代度范围为0.011-1.020,沉降体积范围为0.5-2.5mL,在国内首次用挤压法生产了交联辛烯基琥珀酸木薯淀粉酯,并且为交联辛烯基琥珀酸木薯淀粉酯在食品工业中的应用提供了基础。
具体实施方式
实施例1
称取1500克木薯淀粉,加入20克三偏磷酸钠,1.3克氢氧化钠,加入15克辛烯基琥珀酸酐(用约5倍乙醇将其溶解),然后放在40℃烘箱内将乙醇烘去,加蒸馏水调节水分至30%,混合均匀。将所述物料密封,在40-50℃条件下保温1-2小时。调节挤压条件,螺杆转速90r/min,挤压机三段温度分别为50℃,80℃,100℃。将所述物料放入挤压机内挤压,同时完成交联与酯化反应。反应后对其进行干燥,在室温下冷却,粉碎,置于密封样品袋。
实施例2
称取1500克木薯淀粉,加入25克三偏磷酸钠,1.5克氢氧化钠,加入20克辛烯基琥珀酸酐(用约5倍乙醇将其溶解),然后放在40℃烘箱内将乙醇烘去,加蒸馏水调节水分至30%,混合均匀。将所述物料密封,在40-50℃条件下保温1-2小时。调节挤压条件,螺杆转速150r/min,挤压机三段温度分别为60℃,90℃,130℃。将所述物料放入挤压机内挤压,同时完成交联与酯化反应。反应后对其进行干燥,在室温下冷却,粉碎,置于密封样品袋。

Claims (1)

1.一种交联辛烯基琥珀酸木薯淀粉酯的制备方法,其特征在于以木薯淀粉作为原料,以三偏磷酸钠为交联剂,以辛烯基琥珀酸酐为酯化剂,经过双螺杆挤压机挤压,同时完成酯化和交联反应后,再经干燥、冷却、粉碎而制得;
物料质量配比为木薯淀粉100份,交联剂0.8-2份,酯化剂0.8-1.5份,氢氧化钠0.08-0.1份;
工艺为:按配比称取木薯淀粉,加入交联剂三偏磷酸钠,氢氧化钠,和用辛烯基琥珀酸酐5倍质量乙醇溶解的辛烯基琥珀酸酐溶液,然后放在30-40℃烘箱内将乙醇烘去,加蒸馏水调节水分含量至30%,混合均匀;将所述物料密封,在40-50℃条件下保温1-2小时;调节挤压条件,螺杆转速70-150r/min,挤压机三段温度分别设定为50-60℃,80-90℃,100-130℃;将所述物料放入挤压机内挤压,同时完成交联与酯化反应;反应后在30-40℃对挤出物进行干燥,在室温下冷却,粉碎,置于密封样品袋包装。
CN2010102869367A 2010-09-20 2010-09-20 一种交联辛烯基琥珀酸木薯淀粉酯的制备方法 Expired - Fee Related CN101921342B (zh)

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CN102086233B (zh) * 2010-12-24 2012-10-03 陈明兴 一种木薯变性淀粉及其生产方法
CN102558371B (zh) * 2011-12-29 2014-03-26 江南大学 一种十二烯基琥珀酸淀粉酯的挤压制备方法
CN103224570A (zh) * 2013-05-20 2013-07-31 江南大学 一步挤压制备交联十二烯基琥珀酸淀粉酯的方法
CN103435709B (zh) * 2013-07-26 2016-02-24 广西大学 氧化酯化复合变性淀粉及其制备方法
CN110204622A (zh) * 2019-06-21 2019-09-06 东莞建泰生物科技有限公司 一种交联辛烯基琥珀酸铝淀粉及其制备工艺和在多孔陶瓷中的应用
CN115211566A (zh) * 2022-03-23 2022-10-21 东北农业大学 一种用Pickering o/w乳剂微流化制备橄榄油微胶囊的方法

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