抗静电剂PEE的应用工艺优化

由DMT、EG和PEG合成了抗静电剂PEE,并通过正交试验分析得出了抗静电剂PEE对涤纶进行抗静电整理的较优工艺条件。     

含金属盐亲水性涤纶织物抗静电剂的合成

以对苯二甲酸二甲酯、乙二醇、聚乙二醇(PEG)、己二酸和氧化锌为原料,合成了一种亲水性永久型涤纶织物抗静电剂。研究了PEG的相对分子质量、亲水链段的质量分数与抗静电剂效果之间的关系;探讨了温度、催化剂、真空度和杂质等因素对合成反应的影响。结果表明:PEG的相对分子质量应为3 000,质量分数控制在60%左右;缩聚反应的温度在240℃~270℃,真空度0.089 MPa,三氧化二锑为催化剂;所合成的含金属盐亲水性涤纶织物抗静电剂具有优良的抗静电性和耐水洗性。     

聚乙二醇-聚己二酸酐的合成

采用熔融缩聚法合成了PEG(1)-己二酸酐(2)聚合物。考查了反应温度、反应时间、真空度及物料配比等因素的影响,实验结果表明:在反应温度为200°C,反应时间为90 min,真空度22.7Pa,n(1)∶n(2)=1∶20条件下,聚合物的相对分子质量达6000以上。通过FT IR对合成产物进行了表征。     

三(环氧丙基)异氰尿酸酯的合成

采用2步法合成了三(环氧丙基)异氰尿酸酯(TGIC),研究了物料配比、催化剂、反应时间、反应温度、反应时真空度等对产率的影响,得到了如下工艺条件:采用四甲基氯化铵作催化剂,原料配比为:n(氰尿酸)∶n(环氧氯丙烷)=1∶18;第1步反应时间为6h;第2步反应时间为1 5h;第1步反应温度90℃;第2步反应真空度0 09MPa,产率95%以上。     

聚(癸二酸-聚乙二醇)酸酐的合成研究

采用熔融缩聚法合成了标题化合物。考查了反应温度、反应时间、真空度及物料配比等因素对聚合物相对分子质量的影响。实验结果表明:在反应温度为185℃,反应时间为90 min,真空度为25 Pa,两种预聚物w(产物2)∶w(产物3)=80∶20条件下,聚合物的相对分子质量达9 000以上。通过FT-IR及1HNMR对合成产物进行了表征。     

盾构件聚氨酯止水材料的制备与性能研究

以聚乙二醇(PEG)、聚丙二醇(PPG)、二苯基甲烷二异氰酸酯(MDI)为主要原料,1,4–丁二醇(BDO)为扩链剂,合成出遇水膨胀聚氨酯弹性体。研究了不同相对分子质量的PEG、多元醇配比、预聚体w(NCO)以及异氰酸酯指数(R值)对聚氨酯弹性体性能的影响。结果表明:PEG相对分子质量为1 000,m(PPG1000):m(PEG1000)=20:80,预聚体w(NCO)控制为8%~9%,R值为1.06时,制备的膨胀型聚氨酯止水材料综合性能最好。     

纸品粘结用聚氨酯热熔胶的制备

采用不同相对分子质量的聚乙二醇(PEG)和甲苯二异氰酸酯(TDI)为原料制备了水溶性聚氨酯热熔胶。讨论了PEG相对分子质量、原料配比、TDI滴加温度、反应时间等对产品性能的影响。结果表明,当PEG8000∶PEG600∶TDI摩尔比为1∶1∶2.28、TDI滴加温度为60～70℃、反应时间为3h时,所得聚氨酯热熔胶软化点为72.5℃、剪切强度为2.668MPa、吸湿率为0.81%,胶丝水溶性优,适用于纸品的粘接,并有利于废纸的回收处理。     

聚氨酯丙烯酸酯的合成研究及应用

以IPDI,PEG1000和HEMA为原料合成了可紫外光固化的聚氨酯丙烯酸酯低聚物(PUA),用作凝胶聚合物电解质中的聚合物基体。对合成的产物(PUA)进行红外图谱分析,并讨论了合成过程中反应温度,反应时间,反应物配比等因素的影响。结果表明较佳的合成条件为:n(IPDI):n(PEG1000):n(HEMA)=1:2:2.08,第一步的反应温度在60～75℃,反应时间为2 h;第二步的在55～65℃,时间为2.5 h。     

聚乙二醇硬脂酸酯的合成

以硬脂酸为基本原料,通过酰氯化后所得硬脂酰氯,再与聚乙二醇(400)进行酯化反应合成聚乙二醇(400)硬脂酸酯非离子表面活性剂。探讨了物料配比、反应时间、温度对合成反应的影响。合成反应的最佳条件为:反应温度为100℃,时间为1.0h,硬酯酰氯:聚乙二醇=1.1:1(摩尔比)。     

两步法合成高环氧值低黏度聚丙二醇缩水甘油醚的研究

以氢氟酸为催化剂,环氧氯丙烷(ECH)、相对分子质量为400的聚丙二醇(PPG)为基体,采用两步法合成低黏度聚丙二醇缩水甘油醚。通过对产物环氧值和产率分析,研究了开环原料配比、催化剂用量、温度、时间以及闭环原料比、温度、时间对合成的影响。实验结果表明:催化剂、原料配比、开环反应、闭环反应均对产物环氧值和产率有较大影响。最优反应条件为m(催化剂):m(PPG)=0.15%、m(PPG):m(ECH)=1:2.4、开环温度60~65℃、闭环温度50~55℃,此时环氧值为3.23 mmol/g,收率为95.49%,旋转黏度为36~60 m Pa·s。     

Antielectrostatic poly(ether ester) block copolymer of poly(ethylene terephthalate‐co‐isophthalate)–poly(ethylene glycol)

Poly(ethylene terephthalate) (PET) fiber has a low moisture regain, which allows it to easily gather static charges, and many investigations have been carried out on this problem. In this study, a series of poly(ethylene terephthalate‐co‐isophthalate) (PEIT)–poly(ethylene glycol) (PEG) block copolymers were prepared by the incorporation of isophthalic acid (IPA) during esterification and PEG during condensation. PEG afforded PET with an increased moisture affinity, which in turn, promoted the leakage of static charges. However, PET also then became easier to crystallize, even at room temperature, which led to decreased antistatic properties and increased manufacturing inconveniences. IPA was, therefore, used to reduce the crystallinity of the copolymers and, at the same time, make their crystal structure looser for increased water absorption. Moreover, PET fibers with incorporated IPA and PEG showed good dyeability. In this article, the structural characterization of the copolymers and antistatic and mechanical properties of the resulting fibers are discussed. At 4 wt % IPA, the fiber containing 1 mol % PEG with a molecular weight of 1000 considerably improved antistatic properties and other properties. In addition, the use of PEIT–PEG as an antistatic agent blended with PET or modified PET fibers also benefitted the antistatic properties. Moreover, PEIT–PEG could be used with another antistatic agent to produce fibers with a low volume resistance. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 1696–1701, 2003     

脂肪酸酯类抗静电剂的合成及应用研究

以棕榈酸和回收的聚乙二醇为原料,采用酯化法合成了一种脂肪酸酯类抗静电剂,研究了醇酸摩尔比、催化剂用量、反应时间和反应温度对酯化反应的影响。结果表明,在醇酸摩尔比为1.5:1,催化剂用量为0.8 %,反应时间为5 h,反应温度为140 ℃的条件下,所得产物的综合性能最好。将制备的脂肪酸酯应用于聚乙烯中作为抗静电剂,讨论了其含量、试样放置时间、环境温度对聚乙烯抗静电性能的影响,发现随着脂肪酸酯含量的增加、放置时间的延长和环境温度的升高,抗静电效果提高,当脂肪酸酯含量为3份时,抗静电效果最佳。     

PEG-ZnO-PP复合抗静电剂及其对聚丙烯纤维的改性

选用相对分子质量分别为10 000和20 000的聚乙二醇(PEG 10000,PEG 20000)与氧化锌(ZnO)、马来酸酐(MAH)混合,再与聚丙烯(PP)共混,制备复合抗静电剂(PEG-ZnO-PP),然后将其与PP共混纺丝,制得共混纤维。研究了PEG-ZnO-PP复合抗静电剂的流动性和热性能,考察了共混纤维的力学性能和抗静电性。结果表明:复合抗静电剂的流动性和热性能因PEG的相对分子质量不同而有所不同,含PEG 10000的复合抗静电剂的流动性能较好,且其熔融热焓、熔融结晶温度、结晶放热高于含PEG 20000的复合抗静电剂。共混纤维力学性能和静电半衰期随复合抗静电剂含量的增加而减小,含PEG 20000的共混纤维抗静电效果更好。     

聚酯纤维抗静电母粒的研制

研究了以DMT,EG,PEG为原料,苯磺酸钠等为辅助抗静电剂制备抗静电母粒的工艺。用所制备的抗静电母粒与PET切片按质量比12∶88混料纺丝,制得织物具有良好的抗静电性能,达到了“GB12014-89”中抗静电性能的要求。     

Enhanced dynamic mechanical and shape‐memory properties of a poly(ethylene terephthalate)–poly(ethylene glycol) copolymer crosslinked by maleic anhydride

Dimethyl terephthalate (DMT) and ethylene glycol (EG) were used for the preparation of poly(ethylene terephthalate) (PET), and poly(ethylene glycol) (PEG) was added as a soft segment to prepare a PET–PEG copolymer with a shape‐memory function. MWs of the PEG used were 200, 400, 600, and 1000 g/mol, and various molar ratios of EG and PEG were tried. Their tensile and shape‐memory properties were compared at various points. The glass‐transition and melting temperatures of PET–PEG copolymers decreased with increasing PEG molecular weight and content. A tensile test showed that the most ideal mechanical properties were obtained when the molar ratio of EG and PEG was set to 80:20 with 200 g/mol of PEG. The shape memory of the copolymer with maleic anhydride (MAH) as a crosslinking agent was also tested in terms of shape retention and shape recovery rate. The amount of MAH added was between 0.5 and 2.5 mol % with respect to DMT, and tensile properties and shape retention and recovery rate generally improved with increasing MAH. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 27–37, 2002     

新型抗静电涤纶的研制 Ⅱ.抗静电剂APPS的链结构与抗静电性能的关系及其抗静电机理

研究了抗静电剂ＡＰＰＳ分子中第三单体链段（ＰＳＩＰＥ）含量、ＰＥＧ链段含量及ＰＥＧ链段相对分子质量对ＡＰＰＳ抗静电性能的影响，同时探讨了ＡＰＰＳ的耐水洗性及其耐水洗的原因。利用扫描电子显微镜（ＳＥＭ）观察并分析了抗静电剂ＡＰＰＳ与ＰＥＴ共混后的形态结构和ＡＰＰＳ的抗静电机理。结果表明：ＰＥＴ－ＡＰＰＳ共混体系中二者呈不相容状态，ＡＰＰＳ以网络状均匀分布在ＰＥＴ基体中。ＰＳＩＰＥ链段对ＡＰＰＳ的抗静电效果影响最大，而ＰＥＧ链段含量、相对分子质量对其影响不明显。ＡＰＰＳ的耐水洗性优良而抗静电机理在于吸湿和离子导电的协同作用。     

Surface modification of poly(ethylene terephthalate) film by coating with poly(ethylene glycol)‐grafted polystyrene

The poly(ethylene glycol) (PEG)‐grafted styrene (St) copolymer, which was formed as a nanosphere, was used as an agent to modify the surface of poly(ethylene terephthalate) (PET) film. The graft copolymer was dissolved into chloroform and coated onto the PET film by dip–coating method. The coated amount depends on the content ratios of PEG and St, the solution concentration, and the coating cycles. The graft copolymers having a low molecular weight of PEG‐ or St‐rich content was fairly stable on washing in sodium dodecyl sulfate (SDS) aqueous solution. It was confirmed that the PET surface easily altered its surface property by the coating of the graft copolymers. The contact angles of the films coated with the graft copolymers were very high (ca. 105–120°). The coated film has good antistatic electric property, which agreed with PEG content. The best condition of coating is a one‐cycle coating of 1% (w/v) graft copolymer solution. The coated surface had water‐repellency and antistatic electric property at the same time. The graft copolymer consisted of a PEG macromonomer; St was successfully coated onto PET surfaces, and the desirable properties of both of PEG macromonomer and PSt were exhibited as a novel function of the coated PE film. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 1524–1530, 1999     

PET/PEG共聚酯连续熔融终缩聚过程两相稳态模型分析

针对高性能共聚酯PET/PEG缩聚过程,建立了圆盘反应器中连续熔融聚合两相稳态模型,模拟分析了缩聚反应温度、压力、停留时间以及传质系数对气相组成、共聚酯数均分子量、端羧基浓度以及副产物二甘醇和水浓度的影响。结果表明：挥发组分主要在反应器的前半部分产生,在z > 0.4后气相挥发总量已经很小;乙二醇占气相组成的比例极高,约为90%,而二甘醇的含量极低,只为0.5%左右;随反应器温度、真空度、停留时间、传质系数的增加,共聚酯产物的分子量增大,当传质系数大于0.1 s^-1后,反应器出口的共聚酯分子量几乎不再变化,此时已不受传质控制,最终产物的分子量约26000。     

Hydrolytic depolymerization of poly(ethylene terephthalate) under microwave irradiation

This article covers the depolymerization of poly(ethylene terephthalate) (PET) under microwave irradiation in neutral water. The reaction was carried out in a sealed reaction vessel in which the pressure (or temperature) was controlled. The hydrolytic product contained terephthalic acid, ethylene glycol, and diethylene glycol characterized by IR spectrometry and gas chromatography. The undepolymerized PET was identified by gel permeation chromatography. Both the yield of terephthalic acid and the degree of PET depolymerization were seriously influenced by pressure (or temperature), the weight ratio of water to PET, and the reaction time. The applied irradiation power had little influence on the degree of PET depolymerization. With a pressure of 20 bar (temperature = 220°C), a reaction time of 90–120 min, and a weight ratio of water to PET of 10:1, the PET resin was depolymerized completely. The molecular weight and the molecular weight distribution indicated that the hydrolytic depolymerization of PET obeyed the regular chain‐scission mechanism to some extent. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 95: 719–723, 2005