辛烯基琥珀酸淀粉酯的性能与合成方法

主要叙述了辛烯基琥珀酸淀粉酯的基本性能,用处,以及它的不同合成方法,包括各自的影响因素以及各自的特点.     

有机相法合成辛烯基琥珀酸淀粉酯

变性淀粉工业是国内具有广阔的市场前景的工业之一。辛烯基琥珀酸淀粉酯是种非常重要的亲油脂变性淀粉,乳化稳定,效果优良,对人体无毒副作用,作为一种新的食品添加剂,成为国际上通用的安全添加剂,在各种行业都有广泛的应用。本研究从反应机理出发,以丙酮为分散相,进行反应。探索了多种催化剂,寻找最佳催化剂;通过实验确定以磷酸钠作为催化剂。以此基础上,探索不同浓度的辛烯基琥珀酸酐(OSA)对反应取代度的影响,寻找合适的反应条件。最适宜的反应条件为:OSA反应浓度为0.6 mol/L,需要的丙酮体积为150 mL,磷酸钠质量为7 g,加热温度为40℃,加热时间为4 h。     

辛烯基琥珀酸淀粉糖酯在沐浴露中的应用研究

研究了新型表面活性剂辛烯基琥珀酸淀粉糖酯(OSS)的理化性质及其在沐浴露中的应用。采用吊片法测定OSS的表面张力,结果表明最低表面张力为27.71m N/m,临界胶束浓度(cmc)最低为0.20 g/L,与烷基糖苷(APG)的cmc接近。OSS的亲水亲油平衡(HLB)值为14~16,可以作为O/W型乳化剂。通过凯式定氮法测定OSS的蛋白溶解量研究OSS的温和性,结果表明OSS的蛋白溶解量约0.001 4 g/L,较APG低。OSS与AES复配有一定的协同增效作用,在沐浴露中应用性质温和。     

非晶交联辛烯基琥珀酸淀粉酯的一步法合成及其性能

以非晶木薯淀粉(N-NS)为原料,三偏磷酸钠(STMP)和辛烯基琥珀酸酐(OSA)为变性剂,采用一步法合成非晶交联辛烯基琥珀酸淀粉酯(N-1-COSAS),测定产物的取代度、结合磷含量、透明度、表观黏度、特性黏度和蓝值,并与三步法合成的非晶交联辛烯基琥珀酸淀粉酯(N-3-COSAS)作对比。同时采用傅里叶红外光谱仪(FT-IR)、扫描电镜(SEM)、X射线衍射仪(XRD)和差示扫描量热仪(DSC)对产物的官能团、形貌、结晶结构和热稳定性进行表征。结果表明,N-1-COSAS的取代度、结合磷含量、特性黏度要比N-3-COSAS的大,糊化温度比N-3-COSAS的低;N-1-COSAS与N-3-COSAS在1600 cm–1附近都出现了辛烯基C=C特征吸收峰,表明酯化反应的发生;N-1-COSAS与N-3-COSAS的结晶度均比原淀粉低,峰的弥散程度与N-NS相似;N-1-COSAS与N-3-COSAS颗粒表面比N-NS更加粗糙,且这二者的热稳定性优于N-NS。     

辛烯基琥珀酸淀粉钠的制备及其结构表征

研究了辛烯基琥珀酸淀粉钠(SSOS)的生产方法,并采用红外光谱仪对产品的结构进行了分析。实验结果表明,蜡质玉米淀粉经辛烯基琥珀酸酐(OSA)处理后,产品的取代度为0 017,反映在光谱图上1724cm-1和1565cm-1处产生了新的吸收峰,608cm-1处的吸收峰加强,这些都是OSA基团的特征峰。在制备低黏度SSOS时,α 淀粉酶作用酯化淀粉后产品的DE值(dextroseequivalent)为2 5～6 4,再经糖化酶作用后产品的DE值为14 5～37,可根据最终产品的DE值要求来确定酶的用量以及是否用糖化酶。     

十二烯基琥珀酸淀粉酯的制备及其性质研究

研究了反应温度、反应时间、体系pH、十二烯基琥珀酸酐用量等条件对酯化反应的影响。采用红外光谱对产品进行了结构表征,结果表明反应后淀粉分子上的确引入了烯基琥珀酸酐基团;用扫描电镜观察产品的颗粒形态,发现十二烯基琥珀酸淀粉酯(SSDS)颗粒表面受到一定程度的破坏。研究了SSDS的性质,结果表明SSDS乳化能力强,而且乳化稳定性比较好,SSDS糊符合假塑性流体特征。     

超声作用下辛烯基琥珀酸淀粉酯合成工艺及反应机理研究

以木薯淀粉为原料,辛烯基琥珀酸酐为变性剂,采用湿法工艺,在超声作用下制备辛烯基琥珀酸淀粉酯.用单因素实验探索最佳制备工艺条件及酯化反应机理.结果表明,超声作用制备辛烯基琥珀酸淀粉酯的最佳工艺条件为：超声作用时间30 min,超声功率250 W,酯化pH 8.5,反应温度35℃,在最佳工艺条件下制备所得辛烯基琥珀酸淀粉酯取代度达0.0181,比未施加超声作用所制得的产品取代度提高了28.4％.超声波强化淀粉变性反应机理是超声波的空化效应对木薯淀粉的颗粒结构有一定影响,使淀粉颗粒表面变粗糙,增加了反应物之间的接触面积,强化了酯化反应的发生.     

淀粉辛烯基琥珀酸铝在护肤品中的应用

介绍了淀粉辛烯基琥珀酸铝的结构特点和乳化机理。列举了淀粉辛烯基琥珀酸铝在护肤乳液/霜/膏中的配方,并对各个配方与相应的空白配方进行感官评价测定。结果表明,淀粉辛烯基琥珀酸铝可以增加体系的浓稠度,减轻油腻感,起到改善产品肤感的作用。     

非晶交联辛烯基琥珀酸淀粉酯的制备与结构表征

以木薯淀粉为原料,三偏磷酸钠(STMP)和辛烯基琥珀酸酐(OSA)为变性剂,用乙醇溶剂法合成非晶交联辛烯基琥珀酸淀粉酯(N-COSAS)。以结合磷含量(CP)、取代度(DS)、黏度(η)为评价指标,探讨STMP用量(占淀粉干基的质量分数),交联时间、交联温度、交联p H值和酯化时间、酯化温度、酯化p H值等因素对CP或DS和η的影响。通过单因素和正交试验,得出制备低黏度N-COSAS的较佳工艺条件:在加入STMP 1.5%时,交联反应的时间、温度和p H值分别为4 h,45℃和10.0,酯化反应的时间、温度和p H值分别为3 h、35℃和8.5。扫描电镜观察显示N-COSAS颗粒表面有明显裂痕,表面被卷起;X射线衍射图谱显示,N-COSAS的相对结晶度为8.24%,晶型属于V型;红外光谱显示,N-COSAS在1570.06 cm–1处出现新的吸收峰,在929.69 cm–1处峰的强度增加,证明在淀粉分子中引入了辛烯基琥珀酸基团和交联键。     

高取代度环烯基琥珀酸淀粉酯的合成研究

根据淀粉的结构和性质可以对其进行改性,从而改善淀粉自身的一些缺陷．扩大它的应用范围。琥珀酸淀粉酯是一种重要的变性淀粉,是由烯基琥珀酸酐和淀粉通过酯化反应制得的,其物理化学特性与淀粉相比发生了很大变化,在工业领域得以广泛应用。常用的淀粉酯有辛烯基琥珀酸淀粉酯SSOS和十二烯基琥珀酸淀粉酯SSDS。 合成烯基琥珀酸酐所用的原料一般通过α-烯烃双键异构化的方法获得。由于核算关键异构化产物的平衡受热力学控制,难以在一次平衡中获得α-烯质量分数低于5％的产物。因此必须采用“全异构化”工艺,但是经济成本过高．实施起来比较困难。现以含有共轭双键的山梨酸为原料,以顺丁烯二酸酐（马来酸酐）为亲二烯加成试剂,发生D-A反应制得环烯基琥珀酸酐。这两种原料价格适当,分布合理,是比较理想的原料。     

Edible starch sodium octenyl succinate film formation and its physical properties

Edible starch sodium octenyl succinate (SSOS) films, with or without glycerol as plasticizer, were prepared by solution‐casting method. The effect of SSOS concentration, degree of substitution (DS) of octenyl group, as well as glycerol content, on the properties of SSOS films was studied including tensile strength, water vapor permeability (WVP), and oil permeability (OP). The results indicated that the tensile strength of SSOS film was up to 39.4 ± 1.9 MPa when the concentration of SSOS was 0.05 g/mL and DS was 0.05. The increase of glycerol content resulted in a decrease of film tensile strength. WVP of SSOS films was relatively low. Meanwhile, study in OP showed that SSOS films were oilproof. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

十二烯基琥珀酸淀粉酯的表面性质研究

以直链十二烷基苯磺酸钠（LAS）为参照样,研究了十二烯基琥珀酸淀粉酯（DDSS）表面活性剂的表面张力、硬水稳定性、发泡力及泡沫稳定性等理化特性。结果表明：DDSS具有较好的表面活性,其临界表面张力（γcm）c和临界胶束浓度（cmc）分别为27.786 mN/m和0.49 g/L。DDSS在硬水中具有更好的稳定性,但发泡力和泡沫稳定性较低。DDSS在日化领域具有广泛的应用前景。     

新型表面活性剂琥珀酸单十六酰胺磺酸钠的合成与性能研究

在1,2-二氯乙烷溶剂存在下,十六胺与顺丁烯二酸酐经酰胺化,再与Na2SO3磺化制成了新型表面活性剂琥珀酸单十六酰胺磺酸钠（SHAS）,并用单因素优选法对酰胺化反应条件进行了筛选。得到的最佳反应条件为：十六胺与顺丁烯二酸酐投料物质的量比1：1．18,酰胺化反应温度70℃,酰胺化反应时间20min;顺丁烯二酸酐与亚硫酸钠投料物质的量比1：1．10,磺化反应温度70℃,磺化反应时间3h。目的产物收率〉98％,对SHAS各项应用性能进行了测定。     

Preparation and properties of biodegradable poly(butylene succinate)/starch blends

The vital differences between the use of untreated starch and gelatinized starch in blends with poly(butylene succinate) (Bionolle) were thoroughly examined in this study. The melting temperature decreased slightly with increasing dosages of untreated and gelatinized starch. The added starch perhaps tended to disrupt the intermolecular hydrogen bonding within the Bionolle matrix. On the other hand, a large increase in the crystallinity was seen with the addition of starch. Starch appeared to play a nucleating role in the blends. The trend of the glass‐transition temperature decreasing with the starch level was similar to the trend of the melting temperature. For the same starch content, the glass‐transition temperature showed some variations. For blends containing a certain amount of gelatinized starch, the thermal stability remained to a certain degree but continued to decrease. This was ascribed to the relatively low heat stability of starch. As for the mechanical properties, a significant increase in the tensile strength (up to 2 times) was observed when untreated starch was replaced with gelatinized starch in the blends. Similarly, the tear strength increased up to 1.5 times if gelatinized starch was employed. Apparently, the gelatinization of starch was efficiently achieved for promoting its compatibility with Bionolle. In all cases, the mechanical properties of Bionolle blended with gelatinized starch were better than those of Bionolle blended with untreated starch. A morphological investigation provided evidence in support of these findings. This relatively low‐cost gelatinization approach provides an alternative to a high‐cost compatibilizer approach for improving the performance of biodegradable blends. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 257–264, 2005     

三偏磷酸钠交联对羧甲基淀粉性能的影响

以木薯淀粉为原料,三偏磷酸钠为交联剂,采用溶剂法"一步法"制备了交联羧甲基淀粉,研究了三偏磷酸钠交联对淀粉的溶胀性、特性黏度、分子量及其糊液的黏度、抗酸碱性能、耐温性能、抗剪切性能的影响。结果表明,交联改性降低了淀粉的溶胀性,提高了淀粉的特性黏度和分子量;适度交联能显著提高淀粉糊液的黏度、抗酸碱性能和耐温性能,抗剪切性能也得到有效改善。红外光谱分析(FTIR)证实了木薯淀粉发生了交联反应和羧甲基化反应;X-射线衍射分析(XRD)证实了木薯淀粉经羧甲基化后结晶度降低,交联羧甲基淀粉的结晶度略高于羧甲基淀粉;扫描电镜分析(SEM)证实了交联羧甲基化反应不仅发生在淀粉颗粒表面,也发生在淀粉颗粒内部。交联羧甲基淀粉综合性能优于羧甲基淀粉,可大大拓宽产品的应用范围。     

水溶性辛烯基琥珀酸淀粉酯的三偏磷酸钠改性

以酶解处理后的水溶性辛烯基琥珀酸糯玉米淀粉酯(简称OSS)为原料，三偏磷酸钠为改性剂，制备了改性OSS膜，以膜的抗拉强度为响应值，通过单因素和响应面实验优化了OSS膜的改性工艺，采用³¹PNMR和FTIR对最优条件下制备的膜进行了表征。结果表明，在反应时间5.8 h、pH 6.8、三偏磷酸钠用量为OSS质量的18%的最佳工艺条件下，改性OSS膜的抗拉强度为2.19 MPa，比OSS膜提高了69.77%。改性OSS膜断面均匀，起始相变温度提高14.6℃，归因于三偏磷酸钠和OSS间的氢键键合提高了OSS膜的性能。OSS乳化负载维生素E后再经三偏磷酸钠改性可有效提高乳化膜中维生素E的高温(60℃)贮藏稳定性。     

Effect of surface esterification with octenyl succinic anhydride on hydrophilicity of corn starch films

Surface of corn starch films was modified through esterification using octenyl succinic anhydride as reactant. Physical properties of the films, moisture absorption, and water contact angle were measured to characterize the effect of the surface esterification modification. The influences of the concentration of alkaline aqueous solution for activating starch, reaction temperature, and time were investigated. It was found that the pretreatments with 1.0% or 2.0% NaOH aqueous solution and reacting at 35°C for 6 h gave rise to films possessing higher water contact angle, lower equilibrium moisture content, and moisture absorption rate at 95% relative humidity (RH). After the surface esterification modification, the equilibrium moisture content of the starch film decreased up to 29% at 95% RH and the surface water contact angle of the film increased up to 83%. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Processing and properties of thermoplastic starch and its blends with sodium alginate

Viscosity measurements were carried out on corn starch (CS) and CS–sodium alginate (SA) suspensions at low levels of SA [1 to 10% (w/w)], as a function of temperature. The addition of SA caused the granular CS gelatinization process to occur at a lower onset temperature. CS and CS–SA mixtures were extruded in single‐ and twin‐screw extruders, with 15% glycerol and different water contents. Processing of plasticized CS–SA mixtures required lower temperatures, which is consistent with the viscosity results. Homogeneous and flexible extrudates were obtained by processing in a twin‐screw extruder. Samples in the composition range between 0 and 10% (w/w) SA were examined using tensile tests as a function of water content. Mechanical properties were dependent on the water content and on the SA composition. A significant increase in the Young's modulus value was observed for the blend containing 1% SA. Dynamic mechanical analysis was carried out for CS and CS–SA blends. Two transitions were detected in the temperature range –80 to 150°C. Scanning electron microscopy was used to examine the morphology of the extruded samples. The surfaces of the films were homogeneous, which demonstrated that the CS granules in all samples were characteristically destructured under the conditions used in processing. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 412–420, 2001     

羧甲基淀粉钠的制备

以面粉和氯乙酸为主要原料 ,在NaOH存在条件下加热搅拌合成了羧甲基淀粉钠 ,其最佳投料比为面粉∶氯乙酸∶氢氧化钠 =0 2 5∶0 6∶1(摩尔比 ) ,反应温度为 5 0℃～ 74℃ ,合成出的产品质量好 ,产率高     

Gemini型乙二酰胺琥珀酸己酯磺酸钠的合成研究

以顺丁烯二酸酐、乙二铵、己醇、亚硫酸钠为原料,通过酰胺化反应、酯化反应、磺化反应合成标题化合物.采用单因素优选法优化合成工艺条件.结果如下:1)酰胺化反应:以丙酮为溶剂,顺酐与乙二胺的物质的量比为2.2∶1,回流反应80 min,酰胺化产物产率约96%;2)酯化反应:己醇与乙二胺的物质的量比为2.2∶1,反应温度为130 ℃,反应时间为150 min,酯化率约90%;3)磺化反应:亚硫酸钠与乙二胺物质的量比为:2.2∶1,反应温度为100 ℃,反应时间为3 h,磺化率约90%.IR测定显示终产物为目标产物.表面张力测定结果表明,该产品具有较低的临界胶束浓度与表面张力.