CN1244597C - 热转化淀粉及其制备方法 - Google Patents
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- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
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Abstract
本发明提供了一种处理天然和改性淀粉的有效酸转化方法，相对酸溶液转化方法得到具有低粘度和更高比例较低分子量化合物的产品。该转化淀粉显示出特殊的性能，因此可用于多种产品。
Description
本发明涉及转化淀粉的方法。特别地本发明涉及酸转化方法，从而获得具有低粘度和高含量的低分子量化合物的产品。
因为其中的高分子量聚合物组分，淀粉通常具有良好的增稠性。对于典型地使用具有高淀粉(即固体)含量的应用，例如粘合剂、糖果和食品涂层来说，通常的实践是使用已转化过的淀粉。转化过程导致含降低分子量的聚合物和显现出粘度降低的淀粉产品。
在淀粉工业中最常使用的转化方法包括酸解、氧化、热转化和酶转化。为了便于回收，除了酶转化之外，在改性工艺中使用颗粒淀粉。该回收方法通常包括最终淀粉产品在水中的悬浮液，中和pH，然后滤出淀粉产品并用水洗涤产品。该方法通常要除去盐和带电颗粒(包括在转化过程中产生的低分子量副产物)。
利用上述回收方法在水中转化淀粉的方法是公知的，并在Roy L.Whistler等编辑的“Starch：Chemistry and Technology”，第二版，第十章；M.W.Rutenberg等的Starch Derivatives：Production and Uses，Academic Press Inc.1984中已被公开。
一直需要一种代替的转化方法，可以得到现有技术没有的具有较低粘度和高含量较低分子量化合物的淀粉。
本发明涉及转化淀粉的方法。特别地本发明涉及酸转化方法，从而获得具有低粘度和高含量的低分子量化合物的产品。
本发明方法包括将原料淀粉和酸混合，干燥混合物至基本无水状态，加热干燥的混合物足够长的时间以制备具有漏斗流体粘度为约5至约50秒的转化淀粉。
通过上述方法制备的干燥转化淀粉相对通过传统的含水酸转化方法制备的转化淀粉具有较高含量的低分子量化合物。本发明转化淀粉显示出优异的性能，因此可用于许多产品，包括粘合剂、胶囊基底、甜食和纸张表面上浆剂产品在内。
本发明涉及使用酸转化淀粉，得到具有低粘度和高含量的较低分子量化合物的方法。
所有淀粉类和面粉(其后称为“淀粉”)均可用作原料淀粉，并可衍生于任一天然来源。这里使用的天然淀粉，是在自然界发现的物质。同样适用的是通过标准的育种技术(包括杂交育种、易位、逆位、变型或包括其变体的其他基因或染色体工程等)获得的植物所衍生的淀粉。此外，由人工突变和上述基因组合物的变体而培育的植物所衍生的淀粉在此处也适于用作原料淀粉，其中所述基因组合物的变体可通过突变育种的已知标准方法来产生。
原料淀粉的典型来源是谷物、块茎、根、豆荚和果实。天然来源可以是玉米、豌豆、马铃薯、甘薯、香蕉、大麦、小麦、大米、西米、笕菜红、木薯淀粉、竹芋、美人蕉、高梁及其蜡状或高度直链淀粉的变体。这里使用的术语“蜡状淀粉”拟包括含至少约95wt％支链淀粉的淀粉或面粉，这里使用的“高度直链淀粉”拟包括含至少约40wt％的直链淀粉的淀粉或面粉。
化学改性的淀粉液也可用作原料淀粉。这种化学改性拟包括，但不限于交联淀粉、乙酰化和有机酯化淀粉、羟乙基化和羟丙基化淀粉、磷酰化和无机酯化淀粉、阳离子、阴离子、非离子和两性离子淀粉、丁二酸淀粉和取代的丁二酸衍生物淀粉。改性淀粉的方法是公知的，例如在
Modified Starches：Properties and Uses，Ed.Wurzburg，CRC Press，Inc..Florida(1986).中被公开。
物理改性淀粉也可用作原料淀粉，包括但不限于受热抑制或预凝胶化淀粉。制备受热抑制淀粉的方法例如在美国专利号6221420和其引用的参考文献中被公开，这里引入其公开内容作为参考。制备预凝胶化颗粒淀粉方法的例如在美国专利号4280851、4465702、5037929和5149799中被公开，这里引入其公开内容作为参考。
尽管通过将颗粒淀粉分散在水中，并向混合物中加入酸已制备出通过传统方法酸转化的淀粉，现已发现混合原料淀粉和酸，干燥混合物至基本无水状态，并加热干燥混合物够时间以制备具有漏斗流动粘度为约5至约50秒具有优异性能的淀粉的方法。
基本无水状态是指淀粉混合物干燥至水分含量低于约1％。
一般地，将含水量低于约18％的原料淀粉放入到一个具有对流传导能源的反应器中。这样的反应器包括但不限于流化床、薄层热反应器或装有真空和加热套的加压混合器。然后引入一种流动气体(例如空气)，引入速度使淀粉悬浮在反应床中。将无水酸(例如无水盐酸)和一种载体气体(例如氮气)直接注入流化反应器的流动气体中以实现淀粉和酸的混合。
将流化床的温度升至约50至约135℃。可以用现有技术公知的方法实现升温，所述方法包括，但不限于油加热套或通过热空气源或两种方法联合使用。根据酸化度和原始含水量，反应典型地在约3分钟至约1小时内完成。连续方法典型地需要进行约3分钟至约30分钟。间歇式方法典型地在约30分钟至约1小时内完成。尽管反应基本在少于1小时内完成。但在基本上不劣化最终的转化产品的情况下，可以使用更长的加热时间(例如约6至约8小时或更长)。在反应完成后，冷却反应器倒出淀粉且不需进一步的纯化即可使用。
相反，传统酸溶液转化方法典型地要求约12至约20小时，且要求相对较多的酸以使淀粉进行转化，以及需要额外的纯化和以中和、过滤以及干燥形式进行的加工。由于纯化过程洗掉了低分子量组分，不需纯化的本发明的转化淀粉，相对通过传统溶液方法制备的转化淀粉显示出更高含量的低分子量组分。
通过调整含水量、酸度和反应条件，可以使本发明的有效方法适于生产含不同含量较低分子量组分的转化淀粉。此外，本发明的无水方法使得能以高度控制和可重复方式生产高度转化的淀粉，所述高度转化的淀粉若在水存在下反应的话，则具有不能回收的组分(即传统溶液间歇式加工)。例如可以根据本发明的方法制备淀粉，从而实现不可轻易从水中回收的转化度更高的产品。
通过本发明方法制备的淀粉组合物在确定产品中显示出独特的性能。例如粘合剂和胶囊基底为了达到最佳性能，通常要求加入低分子量低聚糖或向配方中加入糖。本发明的淀粉组合物有利地提供所需的产品，而不需加入低分子量的组分。进而本发明的淀粉可用于要求特殊凝胶和织物的产品，包括例如甜食和纸张表面上浆应用。
下列方法和实施例是为了进一步例举和解释本发明，无论如何不应理解为对本发明的限定。除非另有注释，所有给出的的份数和百分含量是基于重量，全部的温度是基于摄氏度℃。
实施例
在实施例中使用了下述测试方法流体粘度测量
可以用下列方法测量流体粘度(这里也称为漏斗流体粘度)。首先，必须收集淀粉并在烘箱内干燥至含水量低于12％。在测定含水量后，称重不锈钢烧杯和温度计。在蒸馏水中加入19％淀粉，使淀粉和水的总量为300g。在沸水浴内蒸煮混合物15分钟，前5分钟搅拌。后10分钟盖上不锈钢烧杯。蒸煮完成后，将烧杯从沸水浴上移出并冷却至80°F。令烧杯回到与蒸馏水一起蒸煮前的起始重量，并继续冷却至72°F，将烧杯的内容物转移到100ml量筒中。
使用固定孔隙的粘度漏斗测量流体粘度(这里也称为漏斗流体粘度)，和流体粘度是100mL蒸煮物流过孔隙所需时间的量度。测量流体粘度所使用的漏斗是标准58度壁厚的耐热玻璃漏斗，其顶部直径为约9至约10cm，管茎的内径为约0.381cm。漏斗的玻璃管茎切成从尖端起约2.86cm的长度，仔细烧边，用约5.08cm长、外径约0.9525cm的不锈钢喷嘴修整。钢喷嘴在连接到玻璃管茎的顶端处的内径为0.5952cm，流出端内径为0.4445cm，两端之间宽度限制为约2.54cm。钢喷嘴通过Teflon管连接到玻璃漏斗上。校准漏斗，以便允许100mL水在使用上述方法时在6秒内通过。
在漏斗孔隙的上方放置一个指针，将内容物从量筒倒入漏斗。允许少量流回量筒以除去包含的空气。平衡量的内容物倾倒回漏斗，在漏斗上方翻转量筒，并允许内容物从量筒滴入漏斗。从漏斗孔处移去指针，并记录100mL样品流过漏斗尖端所需的时间长度。该时间是淀粉样品的流体粘度。
水流动性的测量
这里使用的水流动性(WF)是根据流动性与粘度成反比，以0-90为尺度所测量的粘度的经验试验。典型地使用Thomas Rotational Shear-type粘度计(商购于Arthur A.Thomas CO.，Philadelphia，PA)测量淀粉的水流动性，其中在30℃下使用粘度为24.73cps的标准油来校准，该油100转要求23.12±0.05秒。通过测量在不同淀粉转化度得到的不同含固量下物质100转所需时间，可以精确并重复测量水流动性。当转化增多时，粘度下降，和WF值增加。
转化淀粉中残留固体的测量
将淀粉(5g)加入到95g水中，并搅拌20分钟。用有凹槽的滤纸过滤浆液。将滤液收集到校正的淀粉折射计的透镜下(用水校准到零)，测量溶解百分数。淀粉颜色的测量(L值)
使用装有石英窗NIR压缩池(商购于Bran-Luebbe，lnc.Buffalo Grove，lll)的Hunter ColorQUEST球型分光光度计(商购于Hunter Associates Laboratory，Inc.，Reston Va)，根据生产商的规程使用下列测量参数测量颜色：范围＝L，观测角＝10，光源＝D65，反射设置＝RSIN，可视面积大小＝LAV和紫外过滤器＝out。
实施例1
热转化淀粉的制备
将用5％环氧丙烷取代的玉米淀粉(4000g，来自National Starch and ChemicalCo)加入到实验室模型流化床干燥器中(直径6英寸，高15英寸，ProcedyneCorporation，New Brunswiok，NJ)。用空气流化淀粉，使得淀粉在流化床中悬浮。
通过分配盘计量加入到流化床中的无水HCl气体(3.1g)。得到pH为2.9的淀粉。通过测量气体钢瓶在将气体送入反应器前后的重量损失来判断HCl的加入量。在加酸前后使用氮气清洁全部管线，以确保与淀粉接触的酸的实际用量。
然后将流入床内的空气温度和床的加热套的温度升至104℃。在1小时后从床中卸出淀粉。所得产品具有15.2秒的漏斗粘度和具有与起始原料相似的白色。
实施例2
比较溶液和热转化的相对效率和产品该实施例例举了与传统溶液转化方法的工艺和产品相比，热转化过程的效率和产品的本性。
根据传统技术，使用淀粉的含水浆液，生产酸转化淀粉。简单的说，在水浴中调节天然木薯淀粉的40％固体搅拌浆液至温度为52℃。直接将浓盐酸加入到浆液中，并搅拌反应混合物14小时。使用碳酸钠调节反应混合物至pH值为4.5，然后使用稀氢氧化钠调节pH值至5.5。所得转化淀粉用水洗涤、滤出溶液并在空气中干燥。利用不同用量的酸，通过“溶液”方法对木薯淀粉进行了三次不同的试验，得到三种具有不同水流动性的转化淀粉(样品A、B和C)。
为了对比，根据实施例1的方法，将三种天然木薯淀粉(样品D、E和F)转化成不同的水流动性。这不需要不同的酸用量。
根据上述方法测量其水流动性(“WF”)、残余固体量和样品A-F的颜色值。所得到的数据列于表1。
表1
| 样品号 | 转化方法 | 使用酸％(基于干淀粉的重量) | WF | 剩余可溶性固体(％) | 颜色(Hunter“L”值) |
| A | 溶液 | 0.7 | 67 | 0.52 | 92.9 |
| B | 溶液 | 1.15 | 77 | 0.79 | 92.4 |
| C | 溶液 | 2.00 | 80 | 1.57 | 92.5 |
| D | 干法 | 0.38 | 78 | 4.10 | 93.0 |
| E | 干法 | 0.38 | 83 | 30.1 | 93.7 |
| F | 干法 | 0.38 | 90 | 79.8 | |
| D | 干法(洗过) | 0.5 | |||
| E | 干法(洗过) | 4.9 | |||
| F | 干法(洗过) | 16.9 |
从表中数据可以看出，本发明的热转化淀粉(根据“干”法制得)相对溶液转化方法(“溶液”)，尽管使用了相对少的酸，但达到了更高的转化度(用相对水流动性来表达)，这证明干法转化方法是更有效的方法。
方法的不同并没有对转化淀粉的颜色赋予负面影响，这可通过比较最终产品的颜色值来证明。进而，可以不须洗涤的情况下使用热转化产品，于是有利地保留含量高得多的低分子量固体。或者可以洗涤热转化淀粉，以控制可溶物的含量程度。
在不脱离本发明的精神和范围的情况下可以作出许多改性和变化，这对本领域的技术人员来说是显而易见的。这里公开的具体实施方式仅是举例，仅由所附的权利要求连同这些权利要求所囊括的等价物的全部范围来限定本发明。
Claims (9)
1.一种转化淀粉的方法，包括：
将原料淀粉和酸混合，
干燥混合物至基本无水状态，和
将干燥的混合物进行加热，加热的温度和时间足以制备具有漏斗流体粘度为5至50秒的转化淀粉。
2.权利要求1的方法，其中在流化床条件下进行该方法。
3.权利要求1的方法，其中加热干燥的混合物少于1小时。
4.权利要求1的方法，其中以间歇式工艺进行该方法。
5.权利要求1的方法，其中以连续工艺进行该方法。
6.一种用权利要求1的方法制得的转化淀粉。
7.一种包含权利要求6所述淀粉的产品.
8.权利要求7的产品，其中该产品选自粘合剂、胶囊基底、甜食和纸张表面上浆剂应用。
9.权利要求6所述的转化淀粉在制备带有特殊凝胶和织物性能的产品中的应用。
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| CA2545327C (en) * | 2003-11-13 | 2013-09-10 | Cerestar Holding B.V. | Method for modifying starch and starch derivatives in a continuous process |
| MX2009002159A (es) * | 2006-08-31 | 2009-03-11 | Kimberly Clark Co | Peliculas biodegradables con alta capacidad para respirar. |
| US8227658B2 (en) | 2007-12-14 | 2012-07-24 | Kimberly-Clark Worldwide, Inc | Film formed from a blend of biodegradable aliphatic-aromatic copolyesters |
| US7998888B2 (en) * | 2008-03-28 | 2011-08-16 | Kimberly-Clark Worldwide, Inc. | Thermoplastic starch for use in melt-extruded substrates |
| US8147965B2 (en) | 2008-05-14 | 2012-04-03 | Kimberly-Clark Worldwide, Inc. | Water-sensitive film containing thermoplastic polyurethane |
| US8338508B2 (en) * | 2008-05-14 | 2012-12-25 | Kimberly-Clark Worldwide, Inc. | Water-sensitive film containing an olefinic elastomer |
| US8927617B2 (en) * | 2008-06-30 | 2015-01-06 | Kimberly-Clark Worldwide, Inc. | Fragranced water-sensitive film |
| US8188185B2 (en) * | 2008-06-30 | 2012-05-29 | Kimberly-Clark Worldwide, Inc. | Biodegradable packaging film |
| US8759279B2 (en) * | 2008-06-30 | 2014-06-24 | Kimberly-Clark Worldwide, Inc. | Fragranced biodegradable film |
| US8329601B2 (en) | 2008-12-18 | 2012-12-11 | Kimberly-Clark Worldwide, Inc. | Biodegradable and renewable film |
| US8283006B2 (en) * | 2008-12-18 | 2012-10-09 | Kimberly-Clark Worldwide, Inc. | Injection molding material containing starch and plant protein |
| US8471003B2 (en) * | 2009-04-14 | 2013-06-25 | Corn Products Development Inc. | Thermally inhibited polysaccharides and process of preparing |
| US8399590B2 (en) * | 2009-10-07 | 2013-03-19 | Akzo Nobel Chemicals International B.V. | Superhydrophilic amphiphilic copolymers and processes for making the same |
| US11173106B2 (en) | 2009-10-07 | 2021-11-16 | Johnson & Johnson Consumer Inc. | Compositions comprising a superhydrophilic amphiphilic copolymer and a micellar thickener |
| FR2992983B1 (fr) | 2012-07-06 | 2014-07-04 | Roquette Freres | Sauces de couchage pour papier et carton contenant une dextrine a teneur elevee en amylopectine |
| FR3024874B1 (fr) | 2014-08-14 | 2016-09-02 | Roquette Freres | Copolymere de dextrine avec du styrene et un ester acrylique, son procede de fabrication et son utilisation pour le couchage papetier |
| US11180575B2 (en) * | 2018-12-28 | 2021-11-23 | Corn Products Development, Inc. | Thermally inhibited starch and process for making |
| BR112020004708A2 (pt) | 2017-09-12 | 2020-09-08 | Corn Products Development, Inc. | composição comestível, método para produção de uma composição comestível, e, amido de mandioca ceroso termicamente inibido |
| JP6853558B2 (ja) * | 2019-02-01 | 2021-03-31 | 鹿児島県 | 加熱処理により特性を改質した低温糊化性でん粉 |
| CN110551225A (zh) * | 2019-10-12 | 2019-12-10 | 广西农垦明阳生化集团股份有限公司 | 一种热粘度稳定性糊精的制备方法 |
| US20230002512A1 (en) | 2019-11-27 | 2023-01-05 | Cargill, Incorporated | Clean label starch compositions |
| WO2023049675A1 (en) | 2021-09-23 | 2023-03-30 | Cargill, Incorporated | Thermally inhibited, ozone treated starch or flour, and a method of manufacturing a thermally inhibited, ozone treated starch or flour |
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| US2845368A (en) * | 1954-05-27 | 1958-07-29 | Staley Mfg Co A E | Dextrinization process |
| GB853828A (en) | 1958-07-21 | 1960-11-09 | Staley Mfg Co A E | Methods for treating starch |
| US3479220A (en) * | 1966-03-24 | 1969-11-18 | Keep Chem Co | Acid-modified starches and flours and method of making the same |
| US3967975A (en) * | 1974-11-25 | 1976-07-06 | Cpc International Inc. | Fluidization apparatus |
| US4280851A (en) * | 1979-12-14 | 1981-07-28 | General Foods Corporation | Process for cooking or gelatinizing materials |
| DD157347A1 (de) | 1981-01-28 | 1982-11-03 | Rolf Schirner | Verbesserung der herstellung von dextrin |
| US4465702A (en) * | 1982-11-01 | 1984-08-14 | A. E. Staley Manufacturing Company | Cold-water-soluble granular starch for gelled food compositions |
| US4510166A (en) * | 1984-01-19 | 1985-04-09 | National Starch And Chemical Corporation | Converted starches for use as a fat- or oil-replacement in foodstuffs |
| US4587332A (en) * | 1984-02-28 | 1986-05-06 | Ogilvie Mills Ltd. | Modified wheat "B" starch for corrugating adhesives |
| DE68914401T2 (de) | 1988-10-07 | 1994-08-25 | Matsutani Kagaku Kogyo Kk | Verfahren zur Herstellung von Dextrin enthaltenden faserigen Nahrungsprodukten. |
| US5149799A (en) * | 1990-01-26 | 1992-09-22 | National Starch And Chemical Investment Holding Corporation | Method and apparatus for cooking and spray-drying starch |
| JPH0728694B2 (ja) * | 1990-02-22 | 1995-04-05 | 松谷化学工業株式会社 | 整腸作用を有する食品組成物 |
| JPH0745521B2 (ja) * | 1990-08-07 | 1995-05-17 | 松谷化学工業株式会社 | 高血圧降下作用を有する高血圧降下剤 |
| US5037929A (en) * | 1990-08-22 | 1991-08-06 | Kansas State University Research Found. | Process for the preparation of granular cold water-soluble starch |
| JPH04173094A (ja) | 1990-11-08 | 1992-06-19 | Matsutani Kagaku Kogyo Kk | 低カロリー・デキストリンの製造法 |
| JP3146086B2 (ja) | 1993-03-24 | 2001-03-12 | 松谷化学工業株式会社 | 鶏飼料 |
| US6221420B1 (en) * | 1993-07-30 | 2001-04-24 | National Starch And Chemical Investment Holding Corporation | Foods containing thermally-inhibited starches and flours |
| US6191116B1 (en) | 1998-04-27 | 2001-02-20 | National Starch And Chemical Investment Holding Corporation | Highly soluble, hydratable, viscous, solution stable pyrodextrins, process of making and use thereof |
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| DE60220599D1 (de) | 2007-07-26 |
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| ES2287207T3 (es) | 2007-12-16 |
| BR0203047A (pt) | 2003-05-27 |
| DK1281721T3 (da) | 2007-09-24 |
| EP1281721A1 (en) | 2003-02-05 |
| ATE364634T1 (de) | 2007-07-15 |
| US20030031775A1 (en) | 2003-02-13 |
| DE60220599T2 (de) | 2008-02-21 |
| EP1281721B1 (en) | 2007-06-13 |
| CN1405186A (zh) | 2003-03-26 |
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