Synthesis of a Novel UV-curable Prepolymer Polypropyleneglycol Diglycidyl Ether Diacrylate

A novel UV-curable prepolymer polypropyleneglycol diglycidyl ether diacrylate （PPGGEA） was synthesized by utilizing polypropyleneglycol diglycidyl ether （PPGGE） and acrylic acid （AA） as starting materials, N, N-dimethylbenzylamine as catalyst and p-hydroxyanisole as inhibitor. The optimum synthetic conditions were in the following： the concentration of N, N-dimethylbenzylamine was 0.80 wt% of reactants, the concentration of p-hydroxyanisole was 0.3 wt% of reactants, the reaction temperature was 90-110 ~C, and the molar ratio of PPGGE to AA was 1：2.2. Meanwhile, 1-hydroxycyclohexyl phenyl ketone of a UV-cured initiator was added to the synthesized PPGGEA to prepare a kind of UV-cured coating. The mechanical properties of the UV-cured films were determined, giving 29.99 MPa of tensile strength, 834.27 MPa of the Young＇s modulus and 5.66% of elongation at tear.

Preparation and Characterization of Carboxyl-terminated Poly(butadiene-co-acrylonitrile)-epoxy Resin Prepolymers for Fusion-bonded-epoxy Powder Coating

Liquid carboxyl-terminated poly（butadiene-co-acrylonitrile）（CTBN）-epoxy resin（EP） prepolymers were prepared with different contents of CTBN.The chemical reactions between EP and CTBN were characterized by Fourier ransform infrared（FTIR） spectroscopy and gel permeation chromatography（GPC）.The scanning electron micrograph（SEM） and dynamic mechanical analysis（DMA） of curing films showed phase separation,and the rubber particles were finely dispersed in the epoxy matrix.Mechanical properties analysis of curing films showed that impact strength and elongation at break increased significantly upon the addition of CTBN,indicating good toughness of the modified epoxy resins.Thermogravimetric analysis（TGA） showed that the incorporation of CTBN had little effect on the thermal stability of EP.Fusion-bonded-epoxy（FBE） powder coatings modified with CTBN-EP prepolymers were prepared.The experimental results demonstrate the ability of CTBN-EP prepolymers,toughening technology to dramatically enhance the flexibility and impact resistance of FBE coatings without compromising other key properties such as corrosion protection.

Synthesis of a Novel UV-curable Prepolymer Hexanediol Diglycidyl Ether Diacrylate and Its Cured Film Tensile Property

A novel UV-curable prepolymer hexanediol diglycidyl ether diacrylate （HDGEA） was synthesized by utilizing hexanediol diglycidyl ether （HDGE） and acrylic acid （AA） as starting materials, N, N-dimethylbenzylamine as catalyst and p-hydroxyanisole as inhibitor. The optimal synthetic conditions were that the concentration of N, N-dimethylbenzylamine was 0.80 wt% of reactants, the concentration of p-hydroxyanisole was 0.3 wt% of reactants, the reaction temperature was 90-110 ℃, and the molar ratio of HDGE to AA was 1︰2.2. Meanwhile, 1-hydroxycyclohexyl phenyl ketone of a UV-curing initiator was added to the synthesized HDGEA to prepare a kind of UV-curing coating. The mechanical properties of the UV-cured films were determined, giving 31.87 MPa of tensile strength, 871.88 MPa of Young＇s modulus and 6.77% of elongation at tear.

Preparation and Characterization of Phenolic Prepolymer Impregnated Chinese Fir by Cyclic Increasing-Pressure Method with Green and Efficient

The Chinese fir wood was impregnated using a cyclic increasingpressure method(CIPM)with phenolic prepolymers as the impregnating modifier.Unmodified Chinese fir and progressive increasing-pressure method(PIPM)impregnated Chinese fir were used as reference samples and were compared and analyzed.The product’s chemical structure,internal morphology,crystal structure,and heat resistance were characterized.The transversal and longitudinal sections showed better filling effects,so that it bore greater external loading and reduced the water storage space.CIPM infused more phenolic prepolymer into the Chinese fir.Not only producing more physical filling but also forming more hydrogen bond associations and chemical bond combinations.Compared with PIPM and unmodi-fied Chinese fir,the CIPM impregnated Chinese fir had better mechanical strength and water resistance.The cellulose chains in CIPM impregnated Chinese fir were more closely linked and their crystallinity were clearly improved.Changes in internal morphology and crystal structure explained the reason why the mechanical properties and water resistance of CIPM impregnated Chinese fir were improved significantly.This Chinese fir had lower thermal decomposition rates,higher decomposition residual rates,and smaller combustion flames,which confirmed that it possessed improved heat and fire resistance.

Performance of CTBN(carboxyl-terminated poly (butadiene-co-acrylonitrile))-EP(diglycidyl ether of bisphenol-A (DGEBA)) Prepolymers and CTBN-EP/polyetheramine (PEA) System

CTBN-EP prepolymers were synthesized from CTBN and epoxy resin under the catalysis of HTMAB. FTIR analyses indicate the formation of ester group between the carboxyl group of CTBN and the oxirane group of epoxy resin. The viscosity of modified prepolymer increases with CTBN content increasing, but the epoxy value of the prepolymer decreases greatly. DSC analyses verify that CTBN affects the curing process of CTBN-EP/PEA system. Mechanical testing presents the improved toughness of CTBN-EP/PEA curings for the decrease of tensile strength, flexural strength and compressive strength, and increase of impact strength and elongation-at-break with the CTBN content increasing. SEM micrographs show the rubber phase with many holes in diameter about 0.5-1.5 μm is formed when CTBN content is lower than 10 phr. However, the pattern of SEM graph shows some stalactite-like strips when CTBN content is higher than 15 phr. Furthermore, the SEM image of 25 phr CTBN sample forms a kind of co-continuous structure.

Chemical Analyses of Palm Kernel Oil-Based Polyurethane Prepolymer

Polyurethane (PU) was prepared from palm kernel oil-based monoester polyol (PKO-p) via prepolymerization method at NCO/OH ratio of 200/100, 150/100, 100/100, and 75/100 at ambient temperature under nitrogen gas atmosphere. The structure of the synthesized prepolymerized PKO-p PU was determined using FTIR and 13C NMR. The disapperance of NCO peak in the FTIR spectrum at 2270 cm–1 - 2250 cm–1 cm showed that MDI has completely reacted to form PU. The appearance of C=O peak at 1700 cm–1 indicated that hydrogen bonding was formed between the soft segmented chain of the PKO-p and the hard segmented MDI. Hence, urethane bond was the main polymeric chain in the PU.

Synthesis of a novel UV-curable prepolymer neopentyl glycol diglycidyl ether diacrylate and its cured film tensile property

A novel UV-curable prepolymer neopentyl glycol diglycidyl ether diacrylate (NPGGEA) was synthesized by using neopentyl glycol diglycidyl ether (NPGGE) and acrylic acid (AA) as starting materials, N, N-dimethylbenzylamine as catalyst and p-hydroxyanisole as inhibitor. The optimum synthetic conditions were taken as follows: The concentration of N,N-dimethylbenzylamine, 0.80% of reactants; the concentration of p-hydroxyanisole, 0.3% of reactants; the reaction temperature, 90-110 ; the molar ratio of NPGGE to AA, 1:2.2. Meanwhile, 1-hydroxycyclohexyl phenyl ketone of a UV-cured initiator was added to the synthesized NPGGEA to prepare a kind of UV-cured coating. Mechanical properties of the UV-cured films were determined, giving 28.75 MPa of tensile strength, 923.82 MPa of Young’s modulus and 5.51% of elongation at tear.

生物基耐高温PA5T/56的高效制备及表征

目前,耐高温尼龙(PA)的生产主要采用“预聚合+固相后聚合”法,然而固相后聚合过程中存在的制备周期长、副反应多等技术难题长期得不到有效解决。笔者以生物基戊二胺(PDA)、对苯二甲酸(TPA)和己二酸(AA)为原料,通过在固相后聚合过程前期加入适量水,高效制备了生物基耐高温PA5T/56。研究了TPA与AA的物质的量比对产物熔点的影响,结果表明当其物质的量比为6∶4时,产物(P64)的熔点为309℃,可以作为耐高温工程塑料使用。考察了固相后聚合阶段用水量、反应温度、保温时间和预聚物粒径对固相后聚合产物相对黏度的影响,确定了优化工艺条件:用水量与设备的体积比为1∶300、反应温度为260℃、保温时间为6h、预聚物粒径<0.1mm。通过傅里叶变换红外光谱仪和核磁共振氢谱确认了产物的分子结构。热性能测试结果表明,P64的熔点为309℃,起始热分解温度为375℃,即样品具有很宽的温度加工区间和良好的熔融加工温度窗口。力学性能测试结果表明,P64拉伸强度为85.7 MPa、断裂伸长率15.4%、缺口冲击强度为5.56kJ/m^(2),这与商品化PA6T共聚物的性能相近,表明该样品可以部分代替PA6T共聚物使用,拓宽了应用领域。

矿用MDI-50型聚氨酯加固材料的制备及性能研究

聚氨酯注浆加固材料在煤矿井下使用过程中需保证其力学强度及降低材料注浆过程的反应温度,因而针对添加阻燃剂和通过化学反应以改变材料结构的阻燃改性方法研究极其重要。为了有效提升聚氨酯加固材料力学性能和阻燃性能,在聚氨酯加固材料B组分中引入异氰酸酯和扩链剂预聚工艺,有效合成MDI-TMP加成物,从而整体提高硬段交联程度。通过红外光谱、万能力学试验机和热重、凝胶渗透色谱研究预聚温度对MDI-50型聚氨酯加固材料力学性能和阻燃性能的影响。研究结果表明:最高反应温度、抗压强度和拉伸强度随预聚反应温度增加而升高,预聚温度为80℃时所制得的聚氨酯加固材料力学性能最佳;极限氧指数主要由阻燃剂添加量决定,预聚体的结构对其影响不大。MDI-50型聚氨酯加固材料的反应速率可调,反应温度上升平缓,凝结后具有较高的力学性能,可满足聚氨酯注浆材料在煤矿加固应用的要求。

聚丙烯生产中细粉生成的原因及对策研究

Spheripol工艺广泛应用于聚丙烯树脂的工业生产,但是其产品中常常含有部分细粉,不仅影响产品质量,而且不利于装置的长周期稳定运行,本文通过查阅文献,结合对聚丙烯装置生产过程的考察,分析了生产过程中细粉产生的原因,并结合生产实际提出了一些有助于降低细粉生成的对策,通过关注催化剂质量、优化催化剂配置和预聚合方案,以及提高原料丙烯纯度等方法有望降低细粉生成,改善产品质量。

聚丙烯催化剂预聚合工艺优化研究

考察了釜式淤浆预聚合对Hypol聚合工艺的影响。实验结果表明，对丙烯催化剂进行预聚合可以改善聚丙烯粒子的形态，减少聚丙烯中细粉（粒径小于200μm）的含量，提高聚阿烯粒子的规整性，提高粒子强度。预聚合度的提高会降低催化剂的初始催化活性，但有利于催化活性的平稳释放。当预聚合温度由10℃升高到40℃时，聚合产率降低。预聚合过程中增加助催化剂（三乙基铝）的用量，可以提高催化剂的催化活性（催化活性存在一个最佳值）。预聚合过程中加入外给电子体，可提高聚丙烯粒子的规整性，减少细粉含量，但降低催化剂的催化活性。预聚合后的催化剂在储存时间10—20h内催化活性衰减最快，最大衰减幅度达到40％。

浇注型聚氨酯弹性体的研制

采用2,4甲苯二异氰酸酯(TDI)、聚醚多元醇或聚酯多元醇、扩链剂等原料通过预聚物法合成了浇注型聚氨酯(PUR)弹性体,分析了柔性链段的分子结构、扩链剂的分子结构及异氰酸酯基的含量等因素对PUR弹性体力学性能的影响。结果表明,以聚己二酸丁二酯为柔性链段、MOCA或TX-2为扩链剂、异氰酸酯基质量分数为5%～5.5%时,所得PUR弹性体具有较好的综合性能。

磺酸型水性聚氨酯分散液的合成与性能

以聚己二酸丁二醇酯二醇、异佛尔酮二异氰酸酯、乙二胺为原料,由自制的乙二胺基乙磺酸钠为亲水性扩链剂,采用预聚体法合成磺酸型水性聚氨酯分散液。研究发现,磺酸型水性聚氨酯分散液固含量高(43.66%),稳定性大于6个月,且性能优于羧酸型水性聚氨酯分散液。

丙烯预聚合工艺的研究进展

综述了有关丙烯预聚合的最新进展,包括新的预聚合工艺及其对聚合过程、聚丙烯(PP)产品性能等的影响以及在“超临界”聚合上的应用等。丙烯预聚合对于PP颗粒形态、主聚合阶段的聚合动力学以及聚合工艺都会产生影响。

多交联体系聚氨酯材料的制备与表征

以聚酯多元醇(PEA)、2,4-甲苯二异氰酸酯(TDI-100)为原料,采用预聚法制备预聚体,将预聚体分成两部分分别以不同比例与扩链剂(MOCA)混合反应,再将两种配料不同的混合物体系混合后浇铸成型,即为多交联体系聚氨酯材料。对其力学性能、耐溶剂性能与均一体系聚氨酯材料的性能进行了比较。结果表明,多交联体系聚氨酯材料的拉伸性能稍有下降,耐撕裂性能明显提高;多交联体系聚氨酯材料的耐溶剂性能也明显提高;DMA测定结果表明,多交联体系聚氨酯材料的玻璃化转变温度降低,微相分离更好,阻尼性能下降。

改性氰酸酯的预聚工艺研究

本文研究酚醛环氧改性双酚A氰酸酯,用于制备热熔预浸料。双酚A氰酸酯和酚醛环氧树脂经过适当预聚后在室温下具有一定的粘附性,可制作出具有室温铺敷性的复合材料预浸料。将金属催化剂二月桂酸二丁基锡(DBTDL)加入改性体系,复合材料成型试验结果表明,DBTDL对树脂体系的预聚工艺有明显的改善作用,树脂体系可用于热熔工艺。

Ti－Mg系载体催化剂预聚合对乙烯气相聚合及产物颗粒形态的影响

研究了Ｔｉ－Ｍｇ系载体催化剂经预聚合与未经预聚合的乙烯气相聚合反应。结果表明，预聚合使催化活性增大、产物堆密度增大、颗粒大小均匀。扫描电镜观察表明，预聚合使催化剂颗粒疏松、多缝隙。预聚物、聚合产物颗粒分别由细小的二级类球形粒子紧密聚集而成，二级粒子则由更细小的一级粒子组成。图象分析测得催化剂、预聚物、聚合产物颗粒平均粒径分别是３３、１６８、２６３μｍ，长短轴之比（Ｄ／ｄ）分别是１．５２４、１．５４０、１．５１４。

DQ预聚合催化剂的研究

用DQ催化剂制备了DQ预聚合催化剂,考察了不同条件制备的DQ预聚合催化剂对丙烯聚合活性、聚合动力学行为及聚丙烯性能的影响。实验结果表明,DQ预聚合催化剂可以改善聚丙烯的颗粒形态,并使聚合动力学曲线更加平稳,DQ催化剂-DQ预聚合催化剂-聚丙烯之间存在良好的复形关系;采用10℃下制备的DQ预聚合催化剂进行丙烯淤浆聚合时得到的聚丙烯颗粒形态最好,采用在20℃下制备的DQ预聚合催化剂进行丙烯淤浆聚合时活性(以每克催化剂计)最高,达到30.4kg/(g.h);预聚合时,n(Al)∶n(Ti)=0.8～2.0时聚丙烯的颗粒粒径较均匀;随预聚合倍数的增大,DQ预聚合催化剂的活性(以每克钛计)提高。

高抗冲聚苯乙烯的研制 Ⅱ 预聚合反应过程及形态结构的研究

考察了各种条件下高抗冲聚苯乙烯(HIPS)的本体预聚合反应和相转变过程。并对采用不同基础胶制备的HIPS产品的形态结构进行了研究,发现低顺式聚丁二烯橡胶改性产品的形态结构在某些方面优于高顺胶体系。

聚氨酯型相变微胶囊的制备及在蚕丝织物上的应用

相变材料及其微胶囊的制备是调温织物的核心技术。以聚氨酯(PU)为壁材,相变石蜡为芯材,合成了聚氨酯型相变微胶囊,并且将其应用于增强蚕丝织物的调温功能。生物显微镜和扫描电镜(SEM)图片显示合成的聚氨酯型相变微胶囊具有良好的表面形貌;激光粒度测试可见微胶囊的颗粒分布均匀,平均粒径为2.78μm;微胶囊的红外谱图证实其中有聚氨酯结构的生成;热性能表征结果显示该微胶囊相变温度和相变焓分别为23.80℃和70.31 J/g。经聚氨酯型相变微胶囊整理后的真丝绸具有较明显的调温效果,其相变温度和相变焓分别为24.28℃和1.82 J/g。