驱蚊微胶囊的制备及对粘胶面料的功能整理

利用青蒿挥发油作为芯材制备不同芯壁体积比的青蒿挥发油微胶囊对粘胶纤维面料进行整理,并通过测试青蒿挥发油微胶囊平均粒径与整理前后面料服用性能与驱蚊效果的变化,分析青蒿挥发油微胶囊作为驱蚊整理剂最佳的芯壁体积比。研究表明,按芯壁体积比为2:1制备的青蒿挥发油微胶囊粒径最小,且使用该比例制备的青蒿挥发油微胶囊整理后的粘胶纤维面料不仅保留了粘胶纤维面料的性能,驱蚊效果也较佳,综合芯壁比为2:1为最佳比例。     

溶剂蒸发法制备高效氯氟氰菊酯微胶囊及性能

以乙基纤维素为壁材、二氯甲烷为溶剂,采用溶剂蒸发法制备了高效氯氟氰菊酯微胶囊。通过单因素实验考察了溶剂质量分数、壁材质量分数、乳化剂质量分数和剪切时间对微胶囊平均粒径的影响,通过以微胶囊平均粒径和未包封率作为评价指标的正交实验L9(34)优选了最佳工艺,并通过SEM、FTIR和HPLC对微胶囊的外观形貌、包覆效果和释放性能进行了表征。结果表明:随着溶剂质量分数增大,微胶囊平均粒径先减小后增大,w(溶剂)=25%时,平均粒径最小。随着壁材质量分数增大,微胶囊平均粒径增大。随着乳化剂质量分数增大,微胶囊平均粒径逐渐减小。固定剪切速率,微胶囊平均粒径随着剪切时间增加而减小。以w(二氯甲烷)=25%、w(乙基纤维素)=0.75%、w(乳化剂)[m(Tween80)∶m(Span20)=5∶1]=2%、剪切时间为8 min的工艺条件下得到的微胶囊外观光滑,形态规则,粒径较小(约19.2μm)且均匀,包封率高达82.8%,且具有较好的缓释性能。     

乳化溶剂挥发法制备放线菌酮微胶囊剂

以聚甲基丙烯酸甲酯为囊壁材料,二氯甲烷为溶剂,水为连续相讨论芯材与壁材比、有机相与水相体积比,乳化剂质量分数及剪切乳化速度对放线菌酮微胶囊剂成囊的影响.研究结果证明成囊的最佳工艺条件:室温条件下,以二氯甲烷溶解放线蒲酮,芯材与壁材的质量比为1:1,有机相与水相的体积比为20:100～25:95,以1.2%羟乙基纤维素(MW:20000)为乳化剂,有机相和水相混合后16000 r/min下高速剪切乳化分散3 min,室温下搅拌直至二氯甲烷完全挥发.在此条件下所得放线菌酮微胶囊剂呈球形,平均粒径约为8.1～8.4 um,包覆率在92.01%以上.     

薄荷油微胶囊的制备及其共混熔融纺丝

以密胺树脂为壁材、薄荷油为芯材制备薄荷油微胶囊并与聚丙烯(PP)进行熔融共混纺丝得到了芳香纤维。通过设计正交试验,获得微胶囊的最佳制备工艺条件为:芯壁质量比2∶3、壁材质量分数8%、乳化剂质量分数0.8%、缩聚时间2 h;所得的微胶囊平均粒径小(4.568μm)、热稳定性好、形貌规整且产率高(63.17%)。以PP为基体制备微胶囊质量分数20%的母粒,再与PP进行共混熔融纺丝,结果表明:当共混物中微胶囊的实际添加质量分数为2.5%时,共混物可纺性好,纤维的强度可达3.4 c N/dtex。在纺丝前后微胶囊的含油率变化不大,纤维中的含油量为14.05 mg/g。     

毒死蜱农药微胶囊剂制备工艺研究

为探讨溶剂挥发法制备毒死蜱微胶囊剂的工艺条件,本研究以聚甲基丙烯酸甲酯为囊壁材料,二氯甲烷为溶剂,水为连续相讨论芯材与壁材比、有机相与水相体积比,乳化剂浓度以及剪切乳化速度对毒死蜱微胶囊剂成囊的影响。研究结果证明成囊的最佳工艺条件:在室温条件下,以二氯甲烷溶解毒死蜱,芯材与壁材的比(w/w)为1∶2,有机相与水相的比(v/v)为15∶105~20∶100,以1.5%羟乙基纤维素(MW:20000)为乳化剂,有机相和水相混合后在15000 r/min下高速剪切乳化分散6 min,在室温下搅拌直至二氯甲烷完全挥发。在此条件下所得毒死蜱微胶囊剂呈球形,平均粒径约为8.5~8.8μm,包覆率在94.52%以上。     

二步法制备亚麻油微胶囊及在自修复涂层中的应用

以亚麻油为芯材,脲醛树脂为壁材,采用二步法制备自修复微胶囊。通过探讨芯壁比、乳化剂用量、pH等对微胶囊形貌及性能的影响,确定了微胶囊的最佳合成工艺。将微胶囊应用到环氧树脂基体中制备自修复涂层,并考察了涂层的力学性能及自修复性能。结果表明,当芯壁比为3:5时,乳化剂用量为1.5wt%,脲醛树脂预聚温度为70℃,终点pH为3.0时,制备的微胶囊呈规则球形结构,平均粒径约为140μm,具有良好的热稳定性。当涂层中微胶囊质量分数为3%时,涂层的力学性能提升幅度较大。     

路面材料自修复微胶囊制备工艺研究

以环氧树脂为囊芯,明胶和阿拉伯胶为囊壁,十二烷基硫酸钠(SDS)为乳化剂合成自修复微胶囊。考察了囊材和芯材的比例、反应时间、体系的pH、乳化剂的用量等因素对自修复微胶囊包覆率影响。确定了制备自修复微胶囊的最佳工艺:即囊材和芯材的质量比为10∶9,加入15 mL质量分数为4%的SDS为乳化剂,在pH低于4.0时持续反应3 h合成包覆率为69.9%的自修复微胶囊。     

壳聚糖/明胶抗菌微胶囊的制备及其应用

为了制备用于棉织物天然抗菌整理剂,以绿苋、龙葵和黄柏的复配提取物为芯材,壳聚糖-明胶为壁材,采用复凝聚法制备抗菌微胶囊。研究了乳化剂含量、剪切速度、pH对微胶囊的外观形态及尺寸的影响;借助扫描电子显微镜、傅里叶红外光谱仪等对样品进行表征;将抗菌微胶囊用于棉织物的整理并测试其抗菌性能。结果表明：初乳中乳化剂质量分数为5%、剪切速度为8000r/min、pH为5.7为最佳制备条件,制得的微胶囊尺寸分布在1480～3580nm且热稳定性良好;当微胶囊质量浓度为25g/L,黏合剂质量分数为5%,热烘温度为40℃,整理试样对金黄色葡萄球菌和大肠杆菌的抑菌率分别为89.30%和81.43%,且抑菌效果持久。     

响应面法优化纳米UF香精微胶囊工艺

采用原位聚合法以脲醛树脂(urea-formaldehyde resins,UF)为壁材制备的微胶囊常在微米级水平上,实验选用吐温80作乳化剂,通过探究实验工艺,制备出了纳米粒径的脲醛树脂香精微胶囊。进行了乳化香精粒径、固含量、壁芯比(UF壁材与香精芯材的质量比,下同)单因素实验,以激光粒度仪测定的微胶囊粒径大小和分布情况为考察指标,确定了3种因素的水平范围。实验表明,当体系固体质量分数小于1%,壁芯比为(2～5):1,乳化香精粒径为50～200 nm时可制得粒径分布均匀的纳米粒径微胶囊。用响应面分析软件进行实验设计,得到了微胶囊粒径与3种因素之间的三次回归模型,其R2值为0.992 7。对模型进行4组实验验证,验证实验结果相对偏差在6%以内,该模型具有较高可信度。     

纳米SiO_2改性脲醛树脂/十二醇相变微胶囊的制备及性能

利用原位聚合法制备了以纳米SiO_2改性脲醛树脂为壁材、十二醇为芯材的相变微胶囊。考察了芯壁质量比、固化终点pH和纳米SiO_2质量分数对微胶囊包封率和芯材质量分数、渗透率的影响,采用扫描电子显微镜(SEM)、差示扫描量热仪(DSC)和热重分析仪(TG)等分别对微胶囊相变材料的表面形貌、粒径和热性能进行了表征。研究结果表明,纳米SiO_2改性脲醛树脂/十二醇相变微胶囊的最佳制备条件为:芯壁质量比为1∶2、固化终点p H=1.5~2、纳米SiO_2质量分数为3%。制备的微胶囊为表面光滑的球形,粒径大小为1.85~5μm,包封率和芯材质量分数分别为62.5%和79.3%,相变潜热为148.4 J/g。     

EFFECTS OF CATALYST AND CORE MATERIALS ON THE MORPHOLOGY AND PARTICLE SIZE OF MICROCAPSULES

In this article, an interfacial polymerization method was employed for micro encapsulation. The wall material was polyurea and the core materials were diethyl (o-) phthalate, dibutyl (o-) phthalate and dioctyl (o-) phthalate. Poly (vinyl alcohol) (PVA) was used as protective colloid and GPE2040 was used as emulsifier. The effects of catalyst in different phases and core materials with different hydrophobicities on the morphology and particle size were studied. It was found that the surface of microcapsules form catalyst in aqueous phase were smoother and the average size was smaller than that with the catalyst in the organic phase and higher hydrophobicity gave smoother morphology.     

Influence of process conditions on the mean size of PLGA nanoparticles

Investigation was carried out to determine the influence of process conditions on the volume mean size of PLGA nanoparticles intended as drug delivery vehicle for an injection formula of protein type therapeutic agent. Nanoparticles were produced by double emulsion-solvent evaporation method to encapsulate bovine serum albumin into the PLGA matrix material. At first aqueous BSA solution was dispersed by sonication into an organic phase composed of dichloromethane as solvent and dissolved PLGA. This first emulsion was dispersed in a second aqueous phase containing PVA emulsifier. Solid nanoparticles were obtained by evaporating the dichloromethane from the droplets. Size distribution of particles was determined by dynamic light scattering. It was found that volume mean particle size was influenced by several process variables, such as PVA concentration in the external phase, PLGA concentration in the organic phase, BSA concentration in the inner phase, volume ratio of the external and intermediate phases, and the time of sonication during the second emulsification. To elucidate their effects a 5-factorial 3-level experimental design and statistical analysis were carried out. Relationship between the mean particle size and process parameters was proposed.     

低皂高稳丙烯酸酯单体细乳液的制备Ⅱ.乳液稳定性机理

在前文研究影响丙烯酸酯细乳液稳定性众多因素的基础上 ,测定加分散相前乳化剂与助乳化剂所形成的复合胶束和加分散相后的细乳液的单体液滴粒径大小及乳液水相乳化剂浓度 ,提出在低乳化剂浓度下制备高稳定细乳液的机理 ,并进一步归纳出制备高稳定细乳液的最佳工艺。     

氨基蒽醌聚氨酯紫色微球粒径调控及形貌

采用1，4-二氨基蒽醌作为发色体，与异佛尔酮二异氰酸酯反应生成紫色预聚物，与聚乙二醇600通过界面聚合法制备了氨基蒽醌紫色聚氨酯微球。考察了乳化剂种类、用量、乳化速度、发色体用量对微球粒径的影响。结果表明：与聚氧乙烯辛基苯酚醚-10、失水山梨醇单油酸酯聚氧乙烯醚（Tween80）和失水山梨糖醇单油酸酯（Span80）相比，十二烷基苯磺酸钠（SDBS）乳化剂更适合用于聚氨酯球的制备。SDBS质量分数3.5%（以油相为基准）的粒径分布最窄，微球粒径在350nm左右。微球平均粒径随乳化速度增大而减小，在8000r/min粒径分布最集中。发色体在壳层体系中加入量为1mmol时粒径分布系数最小，平均粒径在500nm。通过SEM和TEM表征，结果显示：聚氨酯微球粒径在500nm左右，表面光滑的球形，内部呈空心结构。氨基蒽醌聚氨酯紫色微球印花织物颜色性能优异，且具有较高色牢度。     

低温可逆热敏示温微胶囊的粒径控制及结构

采用界面聚合法制备了以CoCl2为芯材、聚乙烯醇为壁材的可逆热敏示温微胶囊,系统研究了乳化剂用量、内水相与油相用量比、搅拌速度、内乳液加入方式对微胶囊粒径的影响,并对微胶囊的结构和形貌进行了表征. 结果表明,当Span-80/Tween-80含量为5%(w)、水油体积比为0.2、转速为1200 r/min、内乳液采用逐步滴加方式加入外水相中时,制备的微胶囊粒径均一,平均粒径为12 mm,分散性好.     

癸酸相变微胶囊的制备及热性能

以尿素、甲醛及癸酸为原料,利用原位聚合法制备了脲醛树脂包覆癸酸的相变微胶囊。以芯壁质量比、乳化剂用量、乳化转速及固化剂含量为变量设计正交实验,采用ESEM、FTIR和DSC分别表征癸酸微胶囊的微观形貌、化学结构及热性能,利用渗漏率实验测试癸酸微胶囊的防渗性能。结果表明,m(OP-10)∶m(Span-80)=4∶1的复合乳化剂有利于改善癸酸微胶囊颗粒特性。癸酸微胶囊P(芯壁质量比3∶2、乳化剂用量占芯材质量5%、乳化转速1400 r/min、固化剂间苯二酚用量占尿素质量12%)在微观形貌上分散良好且大小均一,相变潜热为123.91 J/g,渗漏率和包覆率分别为6.95%和69.7%,与癸酸微胶囊S(芯壁质量比1∶1、乳化剂用量占芯材质量6%、乳化转速1100 r/min、固化剂用量占尿素质量10%)相比,癸酸微胶囊P的渗漏率降低了57.2%,包覆率反而提高了132.3%,具有良好的热性能。     

响应曲面法优化水包油型天然松香乳液的制备

以天然马尾松松香为原料、ONIST APS-350为乳化剂采用常压转相法制备水包油（O/W）型天然松香乳液。考察了乳化剂用量、初始乳化温度、油水比（松香和水质量比,下同）与搅拌速度对O/W型天然松香乳液粒径分布的影响,并通过响应曲面法（RSM）对制备乳液的工艺参数进行模拟与优化。结果表明：制备O/W型天然松香乳液的最佳工艺条件为搅拌速度500 r/min、乳化剂用量9.95%、初始乳化温度112℃、油水比10：31,所得乳液平均粒径为131.1 nm,乳液离心稳定,静置3个月不分层,通过TEM表征发现,这种天然松香乳液颗粒具有核壳结构,其粒径大小与粒径仪测试结果一致。     

Herstellung von styrol-butadien-copolymerdispersionen mit einem speziellen emulgator-initiator-system

A special emulsifier-initiator-system, consisting of a nonionic emulsifier, a small amount of an anionic emulsifier and a large quantity of persulfate, is used for the preparation of poly(styrene-butadiene) dispersions. The particle size is determined by the persulfate and the comonomers in addition to the anionic emulsifier. Acrylamide yields dispersions with the smallest particles. The nonionic emulsifier has an appreciable effect on the particle size only in the absence of the above components. In none of the instances investigated the dependence of the number of particles on the anionic emulsifier corresponds to the Smith-Ewart-theory. It is assumed that the primary particles originate in the aqueous solution and that they consecutively agglomerate. This agglomeration is indicated by the strong dependence of the particle size on the persulfate concentration and on the phase ratio. The nucleation stage is completed at a conversion of 1?2%. The particle growth stage is completed at a conversion of 15?30%, depending on the type of nonionic stabilizer used, at a conversion of 15?18% when using polyethyleneoxide. A high monodispersity is a precondition for the linear conversion-time dependence up to high conversions. The decreasing monomer concentration at a conversion of 30% is equalized by a gel effect leading to linear time-conversion plots. In the absence of a modifier one can see an acceleration at a conversion of some 35% which can be explained by an enhanced gel effect within the homogeneous particles.     

烷基苯磺酸盐Gemini的合成与性能

以十二烷基苯、二氯甲烷、1,2-二氯乙烷、三乙醇胺、NaOH等为原料,经傅-克烷基化反应、磺化及中和反应,合成出4种不同结构的烷基苯磺酸盐Gemini表面活性剂异构体,用FTIR和 1H NMR鉴定了中间产品的结构,用滴体积法测定表面活性剂水溶液25℃时的表面张力,确定了临界胶束浓度（CMC）,并对其在乳液聚合中的应用做了研究。结果表明增加侧链烷基或桥链基碳原子的个数,表面活性剂的CMC和γCMC减小,三乙醇胺中和形成的烷基苯磺酸盐表面张力值最小;随着乳化剂浓度增加,乳胶粒子平均粒径减小,平衡时间缩短,转化率提高。