反应共混制备木薯淀粉马来酸酯的工艺研究

以木薯淀粉为原料,甘油为增塑剂,马来酸酐(MA)为酯化剂,通过密炼机熔融反应共混制备木薯淀粉马来酸酯。研究了密炼时间、温度、转速及马来酸酐加入量对淀粉酯取代度(DS)的影响,并采用FTIR对淀粉酯的结构进行表征。实验结果表明,取代度随着密炼温度的升高和密炼时间的延长而增大,当密炼温度为130℃或密炼时间为12.5min时取代度变化变得比较平缓;随着密炼转速的增大,取代度先增大后减小,转速为70r·min-1时达到最大值;随马来酸酐含量的增加取代度近似呈线性增长。FTIR结果表明马来酸酐成功接枝到淀粉链上。     

高取代度酯化淀粉的制备与工艺研究

采用有机溶剂法制备高取代度淀粉琥珀酸酯。以琥珀酸酐为酯化剂,对淀粉进行酯化改性。经单因素试验法得到淀粉琥珀酸酯的制备条件,采用正交试验法研究淀粉琥珀酸酯制备的最佳工艺条件：反应温度50℃,反应时间5 h,每克活化淀粉催化剂用量1 m L,活化淀粉与酸酐分子的摩尔比为1∶3。在最佳制备条件下,制得取代度为0.40的淀粉琥珀酸酯。     

APAM/淀粉共混薄膜力学性能及粘合强度的研究

以丙烯酰胺(AM)、丙烯酸(AA)和丙烯酰氧乙基三甲基氯化铵(DAC)为共聚合单体,通过水溶液聚合合成两性聚丙烯酰胺(APAM),然后探索了它与淀粉的共混比对纤维粘合强度的影响,研究了这种共混物的薄膜性能。研究结果表明,APAM与淀粉共混后能够明显改善对棉和涤纶纤维的粘合强度,随着APAM用量的增加,对棉和涤纶纤维粘合强度逐渐增大;通过与APAM的共混,能够降低淀粉膜的脆性,对淀粉膜具有增韧作用;并能缩短淀粉膜的水溶时间、增加吸湿率和水溶胀率,有利于纺织退浆。     

淀粉/聚丙撑碳酸酯/马来酸酐酯化淀粉完全生物降解塑料的研究

制备了马来酸酐酯化淀粉,红外光谱分析证明淀粉进行了酯化反应,讨论了影响酯化淀粉接枝率的各种因素,确定了马来酸酐酯化淀粉的最佳反应条件。同时制备了淀粉/聚丙撑碳酸酯/马来酸酐酯化淀粉完全生物降解塑料,研究了酯化淀粉加入量对共混物的力学性能和微观形态的影响。结果表明:加入马来酸酐酯化淀粉后,改善了淀粉和聚丙撑碳酸酯的相容性,共混物的力学性能有很大提高。     

酯化淀粉的制备

本文以马铃薯淀粉为原料,醋酸乙烯酯为酯化剂,制备低取代度醋酸酯淀粉,研究了各反应因素对产品取代度的影响,并以取代度为指标,用单因素试验,确定了其最佳工艺条件,即反应体系pH值10.25,反应温度26℃,反应时间1h,酯化剂用量1g。     

马来酸酐干法酯化淀粉胶黏剂制备及性能研究

采用淀粉和聚乙烯醇经马来酸酐干法酯化制备淀粉胶黏剂,在制备过程中加入一定比例功能内交联剂异氰酸酯调胶制备改性淀粉胶黏剂,并制备胶合板,以达到提高其耐水性目的。本实验通过改变马来酸酐占干基淀粉的质量分数对淀粉胶黏剂的各项性能影响。并对胶黏剂进行物化性能、力学强度及耐水性测试,同时采用热重分析仪(TGA)、傅里叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)、差示扫描量热仪(DSC)进行系统表征。DSC测试结果表明,马来酸酐酯化淀粉降低了淀粉的糊化温度,TGA测试结果表明,马来酸酐酯化淀粉相对于纯淀粉,提高了热稳定性,FTIR表明马来酸酐成功酯化到淀粉分子上,并且缔合作用随着马来酸酐量的增加而增强;SEM扫描表明马来酸酐加入使淀粉发生了酯化反应,提高胶合板的胶层的连续性,马来酸酐酯化淀粉同时也提高淀粉胶粘剂胶合板的胶合强度f。     

高取代度淀粉醋酸酯的制备研究

本文就高取代度淀粉醋酸酯的制备进行了研究 ,讨论了原料的选择处理及制备过程中各因素的影响 ,为确定最佳的合成条件提供了依据。结果表明 ,选用优质淀粉原料并进行一定的改性处理 ,以对甲苯磺酸作催化剂 ,合理选配酯化剂 ,预先糊化并控制在低温反应 ,可获得性能优良且性价比较高的高取代度淀粉醋酸酯制品     

正交优化制备酯化淀粉

以马铃薯淀粉为原料,醋酸乙烯酯为酯化剂,制备低取代度醋酸酯淀粉。研究了各反应因素对产品取代度的影响,用正交试验,确定了其最佳工艺条件,即反应体系pH值10.5~11.5,反应温度26℃,反应时间1 h,酯化剂用量1.5 g。     

淀粉磷酸单酯的微波合成研究

用玉米淀粉和磷酸氢二钠及磷酸二氢钠的混合盐反应制备淀粉磷酸单酯,酯化反应在微波条件下进行。 本文探讨了磷酸盐用量、pH值、微波辐射功率、微波辐射时间等因素对取代度的影响。     

木质素马来酸酯的制备研究

以碱木质素和马来酸酐为原料,在乙二醇二甲醚介质中通过体系回流反应制备马来酸酐改性木质素。利用FTIR确认了产物结构,建立了木质素马来酸酯产物中马来酸含量测定的方法。探索了反应时间、马来酸酐的用量等因素对反应的影响,优化实验条件为:反应温度85℃;反应时间6 h;马来酸酐的用量为木质素的40%。在优化条件下,产物收率为94.9%,木质素马来酸酯产物中马来酸官能团质量为木质素的1.25%。     

Effects of starch maleation and sulfosuccination on the adhesion of starch to cotton and polyester fibers

Acid-treated cornstarch was maleinated with maleic anhydride or then further sulfonated with sodium bisulfite to prepare maleinated and sulfosuccinylated starches, respectively. Effects of the sulfosuccination and maleation on the adhesion of starch to cotton and polyester fibers were investigated for warp sizing. The adhesion was evaluated in terms of specific adhesion strength measured with a standard method (FZ/T 15001-2008). Experimental results showed that both sulfosuccination and maleation of cornstarch were able to improve the adhesion of starch to cotton and polyester fibers. In addition, the sulfosuccination and maleation was capable of reducing static contact angles of cooked starch pastes onto the surfaces of cotton and polyester fabrics. Starch sulfosuccination was superior to the maleation in raising the adhesion. The measurements of the biological oxygen demand within 5?days and chemical oxygen demand indicated that both sulfosuccination and maleation did not adversely affect aerobic biodegradation of starch in the ranges of modification level considered. Low level of sulfosuccination could be adopted to improve the adhesion of starch to fibers for warp sizing.     

Carbamoyl ethylation of starch for enhancing the adhesion capacity to fibers

The influence of starch carbamoylethylation upon the adhesion capability of starch to pure cotton, all polyester, and polyester/cotton blend fiber substrates were investigated. The carbamoylethyl starch was prepared by the reaction of starch with acrylamide in an aqueous dispersion. The capability was evaluated in terms of the maximum strength and work‐to‐break of a roving impregnated with the starch pastes. The mechanical behaviors of the adhesive layers were estimated through a method by casting starch films and then by measuring their behaviors under controlled condition. It was found that the carbamoylethylation is an effective means for enhancing the adhesion of starch to fibers. No matter what type of the fibers is used, the adhesion capability obviously enhances compared with those of unmodified starch, even if the degree of substitution is at a very low level. The capacity increases steadily as the modification extent increases. Moreover, the experimental results are also discussed and analyzed especially through the failure type, internal stress, stress concentration, and mechanical behaviors of the adhesive layers among fibers. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Interfacial adhesion reaction of polyethylene and starch blends using maleated polyethylene reactive compatibilizer

The interfacial reaction of the polyethylene (PE)/starch blend system containing the reactive compatibilizer maleated polyethylene (m‐PE) was directly characterized by Fourier transform infrared (FTIR) spectroscopy. A significant amount of anhydride groups on m‐PE existed as hydrolyzed forms, resulting in a large amount of carboxyl groups. Using a vacuum‐heating‐cell designed in the laboratory, the carboxyl groups were successfully transformed into the dehydrolyzed state (i.e., anhydride group). This result enabled the direct spectroscopic observation of chemical reaction occurring at the interface. For the PE/starch blend system containing m‐PE, the chemical reaction at the interface was verified by the evolution of ester and carboxyl groups in the FTIR spectra. The effect of the reactive compatibilizer on the interfacial morphology was also examined by scanning electron micrography (SEM). Enhanced interfacial adhesion was clearly observed for the blend system containing reactive compatibilizer. Tensile strengths of blend systems containing m‐PE also increased noticeably compared with the corresponding system without compatibilizer. A similar observation was made for the breaking elongation data. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 767–776, 2002     

Effect of amphoteric grafting branch on the adhesion of starch to textile fibers

Starch-g-poly(2-methacryloyloxyethyl trimethyl ammonium chloride-co-acrylic acid) (starch-g-P(DMC/AA)) with different zeta potentials was prepared via the graft copolymerization of acid-thinned cornstarch (ATS) with 2-methacryloyloxyethyl trimethyl ammonium chloride (DMC) and acrylic acid (AA) in aqueous medium using Fe²⁺–H₂O₂ initiator. The investigation was carried out to reveal the influence of amphoteric branches grafted onto starch chains upon the adhesion of starch to textile fibers. Zeta potential of starch-g-P(DMC/AA) was adjusted by altering the mole ratio of DMC to AA charged into the copolymerization system. The adhesion was evaluated in terms of bonding strength and specific bonding strength of slightly sized roving based on a legal method (FZ/T 15001-2008) through the comparison of the amphoteric branch-grafted starch with ATS, starch-g-PAA, and starch-g-PDMC for warp sizing. It was found that the charged branches grafted onto starch chains were able to significantly enhance the adhesion. Zeta potential, depending on the mole ratio of DMC to AA units in the grafting branches, showed evident effect on the adhesion and desizability of the grafted starch. Increase in the potential favored to improve the adhesion, but disfavored the removal of the starch from sized warps. Alkali-oxidant agent desizing test confirmed that the starch-g-P(DMC/AA) with neutral potential was desizable. The amphoteric branch-grafted starch exhibited potential application as size base materials in warp sizing operation if its zeta potential was neutral.     

Grafting starch nanocrystals onto the surface of sisal fibers and consequent improvement of interfacial adhesion in sisal reinforced starch composite

Starch nanocrystals (SNCs) were obtained by the hydrolysis of waxy starch and used to improve the interfacial adhesion of a composite of sisal fibers and starch. Sisal fibers were first treated with acrylic acid (AA), and the modified fibers were then reacted with SNCs to form ester groups. The grafted fibers were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The FTIR and XPS results showed that the SNCs were successfully grafted onto the surface of SF-AA, and an ester linkage was formed during the reaction of AA with the SNCs. The SEM analysis showed that the SNCs were distributed over the fiber surface. Tensile tests and pull-out tests were also performed utilizing a two-parameter Weibull distribution analysis to study the effect of the grafted SNCs on the mechanical and interfacial properties. Compared to the untreated fibers, the interfacial shear strength of the grafted SNCs fibers increased by 79.3%. Therefore, the structural similarity between starch and the SNCs contributed towards their compatibility and improved interfacial properties, with the introduction of SNCs being used as an alternative material for fiber surface modification. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47202.     

高取代度羧甲基淀粉的制备

用玉米淀粉、氯乙酸和氢氧化钠为原料，在乙醇溶剂中反应制备了取代度为０．６的羧甲基淀粉。采用正交设计试验考察了物料配比、反应温度、反应时间对产物取代度的影响，确定了最佳反应条件。     

Amphiphilic starch with 3-(trimethylammonium chloride)-2-hydroxypropyl and octenylsuccinyl substituents for strong adhesion to fibers

Amphiphilic starch derivatives with oleophilic octenylsuccinyl (OS) and hydrophilic 3-(trimethylammonium chloride)-2-hydroxypropyl (TMACHP) substituents were derived by the quaternization of acid-treated maize starch with N-(3-chloro-2-hydroxypropyl) trimethylammonium chloride followed by the octenylsuccinylation with octenylsuccinic anhydride. Two series of amphiphilic starches with differential degrees of substitution (DS) and mole percentages of OS to the total substituents introduced onto the starch were characterized by elemental analysis, chemical titration, and FTIR spectroscopy. The effects of the DS and mole percentage on the adhesion of the starch to fibers were investigated using a legal method (FZ/T 15001-2008). The modification was able to significantly improve the adhesion of starch to cotton and polyester fibers due to the reduced surface tension of the cooked starch paste. The adhesion depended not only on the DS of OS and TMACHP substituents, but also on the mole percentage of the OS. The amphiphilic starch had superior adhesion to acid-treated and TMACHP-functionalized starches. The adhesion of the amphiphilic starch was found to reach its maximum at a mole percentage of 70.6% OS. An increase in the total DS reduced the surface tension and favored adhesion, but disfavored reaction efficiency. Based on the adhesion and reaction efficiencies, the amphiphilic starch with a total DS in the range of 0.029–0.051 and a mole percentage of 70.6% OS showed potential for use in warp sizing.     

高取代度淀粉醋酸酯的合成及表征

采用活化淀粉作为原料,醋酸酐作为酯化剂,浓硫酸作为催化剂,在冰醋酸溶剂体系中合成了高取代度淀粉醋酸酯,通过正交实验探讨了各因素与取代度的关系。实验发现,淀粉活化预处理有利于高取代度淀粉醋酸酯的合成;醋酸酐用量是影响淀粉醋酸酯取代度的主要因素,反应温度和催化剂用量是次要因素;最佳反应条件:活化淀粉15.87 g,反应温度70℃,醋酸酐用量28 g,催化剂浓硫酸用量0.7 g,在此条件下制得的淀粉醋酸酯的取代度DS=2.465。通过扫描电镜对淀粉醋酸酯与淀粉的结构进行了观察,发现其聚集态与原淀粉相比发生本质改变,表面疏松多孔,比表面积增大,因此产品具有较好的溶剂溶解性能。