（苏州大学材料与化学化工学部，先进功能高分子材料国家地方联合工程实验室，江苏 苏州 215123）
【摘 要】以丙烯酸丁酯、苯乙烯和其他功能单体为主要组分，采用半连续乳液聚合法，制备了一款低黏度苯丙共聚物乳液（SAEP）。通过正交试验法探索了聚乙烯醇种类、钙粉粒径以及固化剂用量对SAEP胶粘剂性能的影响。研究结果表明：采用聚乙烯醇BP17，钙粉粒径为12 μm，w(固化剂)=13%时，SAEP胶粘剂的实际开放期能达到70 min以上；SAEP胶粘剂的最大干剪切强度为16.6 MPa，热水浸渍法测得的胶粘剂的湿剪切强度高达7.1 MPa，而反复煮沸法测得的剪切强度也可达5.5 MPa。在相同的配方条件下，与经典的市售EP4乳液相比，SAEP与EP4乳液配制的胶粘剂开放期（“胶液静态流动性判定法”）相当，最大干剪切强度几乎一致，但SAEP胶粘剂具有更高的湿剪切强度。
【关键词】高性能木工胶粘剂；苯丙共聚物乳液；聚醋酸乙烯酯乳液；聚乙烯醇
(1.河南工业大学理学院，河南郑州 450001；2.中国科学院海洋新材料与应用技术重点实验室，中国科学院宁波材料技术与工程研究所，浙江宁波 315201)
【摘 要】水下粘接环境的复杂性导致水下胶粘剂的发展面临更多的挑战。如何快速有效地破坏界面水合层的同时，实现胶粘剂与被粘接界面强力粘接，是目前水下胶粘剂面临的两大困难。在本研究中，通过光引发自由基共聚的方式制备了甲基丙烯酸苄基酯（BMA）和[1-乙基-3-甲基咪唑双三氟甲磺酰亚胺盐][甲基丙烯酰氧乙基三甲基铵盐]（[MATA+][TFSI-]）无规共聚物，并通过引入离子液体的策略构建了具有多重相互作用的聚合物/离子液体复合物。通过改变两种单体的物质的量之比以及离子液体的含量，实现了对其杨氏模量、断裂强度和断裂韧性的可控调控。该聚合物/离子液体复合物内部丰富的多重相互作用可以实现在水下对多种物质表面的强力粘接，包括金属（不锈钢、金属铝）、无机非金属（玻璃）、极性聚合物（聚酰亚胺）和非极性聚合物（聚丙烯、聚四氟乙烯）等多种类型的基底，其中与不锈钢的粘接强度达到了250 kPa，远高于其他报道的水下胶粘剂的粘接强度。本研究提出的构建多重相互作用策略对发展水下胶粘剂具有一定的指导意义。
【关键词】离子凝胶；水下粘接；胶粘剂；粘接强度；物理相互作用
赖嘉棋1，管 超1，朱云峰1,2，周 建2，颜玉荣2
（1.江苏理工学院化学化工学院，江苏常州 213001；2.苏州湘园新材料股份有限公司，江苏苏州 215001）
【摘 要】采用3-巯丙基三甲氧基硅烷制备了硅烷改性单组分湿固化聚氨酯胶粘剂（SPU）。采用红外光谱、核磁共振氢谱、凝胶渗透色谱和扫描电子显微镜分析了SPU胶粘剂的结构，使用万能电子试验机、邵氏A硬度计测定了硅烷含量对SPU胶粘剂的力学性能、粘接性能与硬度的影响。研究结果表明：3-巯丙基三甲氧基硅烷成功反应到聚氨酯分子链上，减少了体系中异氰酸根（—NCO）的含量；随着硅烷用量的增加，SPU胶粘剂的拉伸强度与拉伸剪切性能升高，硬度降低，表干时间延长；当硅烷用量为理论用量的110%时，SPU胶粘剂的拉伸强度和拉伸剪切强度分别达0.58、0.72 MPa，比纯PU胶粘剂分别提高了7.41%、63.64%；SPU胶粘剂固化时产生的气泡显著减少，外观明显改善。
【关键词】单组分聚氨酯胶粘剂；硅烷改性；气泡；力学性能；拉伸剪切强度
PE-g-MAH粘接剂的制备及其在阻隔膜中的粘接性能研究
（1.辽宁大学化学院，辽宁沈阳 110036；2.沈阳科通塑胶有限公司，辽宁沈阳 101142)
【摘 要】采用双螺杆熔融挤出法制备了马来酸酐接枝聚乙烯（PE-g-MAH）。探讨了在以基体树脂为线型低密度聚乙烯（LLDPE）的基础上，添加不同种类引发剂含量、不同接枝单体马来酸酐（MAH）含量对制备出PE-g-MAH的性能的影响。同时也探究了不同接枝率、熔融指数以及晶点个数的PE-g-MAH粘接剂在乙烯-乙烯醇共聚物（EVOH）阻隔膜上粘接性能的影响。通过傅里叶变换红外光谱对接枝产物进行定性表征并分析接枝物接枝率，通过熔体流动速率测试分析其流动性，通过180°剥离强度测试分析粘接剂的性能。研究结果表明：当引发剂为过氧化二异丙苯（DCP）且添加0.05份，MAH添加1份时，PE-g-MAH接枝率为0.68%，熔融指数为0.94 g·(10min)-1，晶点个数为12，此时材料粘接性能最佳；选择EVOH作为阻隔层粘接，当接枝率为0.68%时，PE-g-MAH的剥离强度达到最大值为69.0 N/cm，PE-g-MAH粘接剂的粘接性能达到相对最佳。
【关键词】马来酸酐；粘接剂；过氧化二异丙苯；剥离强度；乙烯-乙烯醇共聚物
[康达新材料（集团）股份有限公司，上海 201419]
【摘 要】以聚酯多元醇、聚醚多元醇和二苯基甲烷二异氰酸酯为原料，合成了端—NCO预聚体。同时使用热塑性树脂、增黏树脂等助剂，制备了应用于家电电机密封的反应型聚氨酯热熔胶。考察了异氰酸酯指数、多元醇结构和热塑性树脂种类对其性能的影响，并通过红外光谱法、同步热分析法和电子万能试验机对其分子结构、热性能和机械性能进行了表征。研究结果表明：当异氰酸酯指数范围为1.7~2.1，聚酯/聚醚物质的量比为2∶1，热塑性树脂的添加量为20%时，制备的反应型聚氨酯热熔胶的各项物理性能以及对不同镀锌铁、铝的粘接性能良好，具有优异的耐高低温、耐水耐腐蚀性能，符合工业化快速流水线的操作要求，可用于家电电机密封。
李桢林1,2，胡彬扬2，张雪平1,2，陈文求1,2，范和平1,2
（1.华烁科技股份有限公司，湖北武汉 430074；2.江汉大学湖北省化学研究院，湖北武汉 430056）
【摘 要】选择电子级玻纤布为支撑载体，浸入以耐高温环氧树脂为主体树脂的胶粘剂中，制备出一种综合性能优良的半固化片。通过对所制备的半固化片的粘接强度、回流焊、热应力、介质电阻、介质耐电压、介电常数、溢胶量和热膨胀系数等测试项目进行系统研究。研究结果表明：所制备的高性能不流动半固化片具备优良的性能，能够满足下游客户生产刚挠结合板的需求。
【摘 要】采用螯合型离子交换树脂处理氟化工脱氟后的高盐废水中钙离子（Ca2+）。考察了树脂对Ca2+在静态吸附和动态吸附过程中的主要影响因素和吸附性能，并对多次吸附-再生后的树脂吸附性能进行测试。研究结果表明：树脂对Ca2+最大静态吸附量为35.1 mg/g；当废水NaCl浓度为150.0 g/L时，树脂Ca2+吸附量仅降低5.2%，树脂耐盐性较好；pH对树脂吸附Ca2+的静态和动态吸附量影响较小；动态吸附过程中，随着流量增大，工作吸附容量逐渐减少，适宜的流速应在4~9 BV/h；饱和吸附后树脂充分再生情况下，工作吸附容量基本保持不变。
（深圳先进电子材料国际创新研究院，中国科学院深圳先进技术研究院，广东深圳 518100）
【摘 要】本文综述了导热胶粘剂的传热与粘接的基本机理和模型。分析总结了近年来导热胶粘剂的导热增强技术发展情况。着重介绍了环氧导热胶粘剂以及有机硅导热胶粘剂，并探讨了新材料技术对导热胶粘剂的影响。最后对导热胶粘剂现阶段遇到的问题以及未来可能的研究方向进行了展望。
【关键词】导热胶粘剂；热界面材料；导热系数；热阻；环氧；有机硅；自修复材料
（1.北京化工大学材料科学与工程学院，北京 100029；2.山东鑫龙宇新材料科技有限公司，山东济宁 272622）
【摘 要】印刷包装领域用复合胶粘剂的水性化已有25年的历史。在这25年的发展历程中，从最初的几家公司发展至2006年的数十家，再经10余年的发展，与其他乳液聚合产品一样逐步形成了垄断局面。纸塑复合领域基本被8家公司所垄断，塑塑软包装用水性复合胶粘剂基本由5家公司所垄断。本文就印刷包装用复合胶粘剂的现状及未来发展进行综合评述，并就目前国内印刷包装领域用丙烯酸酯乳液复合胶粘剂所用的交联技术在不同使用场所存在的可能问题提出了有效的解决途径。
【关键词】乳液聚合；复合胶粘剂；制备；技术瓶颈；现状；未来发展
邓 娟1,2，高 燕1,2，梁 彬1,2，李吉明3，王昌勇3
(1.广州机械科学研究院有限公司，广东广州 510700；2.国机智能科技有限公司，广东广州 510700；3.苏州艾迪亨斯胶粘技术有限公司，江苏苏州 215101）
【摘 要】伴随新能源汽车产业在国内的火爆发展，针对动力电池用双组分聚氨酯结构胶的开发研究工作越来越多。本文搜集并整理了近年来国内关于动力电池用双组分聚氨酯结构胶的公开报道、研究进展及行业技术要求，主要性能研究包括阻燃性、导热性、耐老化性、对PET粘接适用性以及可拆卸型。最后对未来发展进行了展望。
【关键词】动力电池；双组分；聚氨酯；结构胶；发明专利；技术要求
Scientific Research Report
Preparation and characterization of high performance waterborne wood adhesive
(College of Chemistry, Chemical Engineering and Materials Science of Soochow University, National and Local Joint Engineering Laboratory of Advanced Functional Polymer Materials, Suzhou 215123, Jiangsu, China)
【Abstract】A kind of low viscosity styrene-acrylate copolymer emulsion (SAEP) was prepared by semi-continuous emulsion polymerization with butyl acrylate, styrene and other functional monomers as main components. The effects of the type of polyvinyl alcohol, the particle size of calcium powder and the amount of curing agent on the properties of SAEP adhesive were investigated by orthogonal experiment. The research results showed that when polyvinyl alcohol BP17 was used, the particle size of calcium powder was 12 μm, and w(curing agent)=13%, the actual pot life of SAEP adhesive could reach more than 70 min. The maximum dry shear strength of SAEP adhesive was 16.6 MPa, the wet shear strength of the adhesive measured by hot water immersion method was up to 7.1 MPa, and the shear strength measured by repeated boiling method was also up to 5.5 MPa. Under the same formulation conditions, compared with the classic commercial EP4 emulsion, SAEP had a similar pot life (static fluidity determination method of emulsion) to EP4 emulsion, and the maximum dry shear strength was almost the same, but SAEP adhesive had higher wet shear strength.
【Keywords】high performance wood adhesive; styrene-acrylate copolymer emulsion; polyvinyl acetate emulsion; polyvinyl alcohol
Study on synergistic enhancement of underwater adhesive by multiple interactions
Sun Zaizheng1,2, Fan Zhiqin1, Mao Dongsheng2, Chen Haiming2
(1.School of Sciences, Henan University of Technology, Zhengzhou 450001, Henan, China; 2.Key Laboratory of Marine Materials and Related Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, Zhejiang, China)
【Abstract】The complexity of underwater bonding environment has led to additional challenges in the development of underwater adhesive. How to quickly and effectively destroy the interface hydration layer and realize the strong bonding between the adhesive and the bonded interface are two major difficulties faced by underwater adhesive at present. In this study, the random copolymers of benzyl methacrylate (BMA) and [1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl) imide][methacryloxyethyl trimethylammonium salt] ([MATA+][TFSI-]) were prepared by photoinitiated free radical copolymerization, and the polymer/ionic liquid complex with multiple interactions were constructed by the strategy of introducing ionic liquid. By changing the mass ratio of two monomers and the content of ionic liquid, Young's modulus, fracture strength, and fracture toughness could be well controlled. The rich multiple interactions within the polymer/ionic liquid complex enabled strong bonding under water to a wide range of material surfaces, including metals (stainless steel, metallic aluminum), inorganic non-metals (glass), polar polymers (polyimide) and non-polar polymers (polypropylene, polytetrafluoroethylene), and other types of substrates, among which the bonding strength to stainless steel reached 250 kPa, which was much higher than those reported for other underwater adhesive.
【Keywords】ionic gel; underwater bonding; adhesive; bonding strength; physical interaction
Effect of silane modification on properties of one-component moisture curing polyurethane adhesive
Lai Jiaqi1, Guan Chao1, Zhu Yunfeng1,2, Zhou Jian2, Yan Yurong2
(1.School of Chemistry and Chemical Engineering, Jiangsu University of Technology, Changzhou 213001, Jiangsu, China; 2.Suzhou Xiangyuan New Materials Co., Ltd., Suzhou 215001, Jiangsu, China)
【Abstract】Silane-modified one-component moisture curing polyurethane adhesive (SPU) was prepared with 3-mercaptopropyl trimethoxysilane. The structure of SPU adhesive was analyzed by infrared spectroscopy, nuclear magnetic resonance hydrogen spectroscopy, gel permeation chromatography and scanning electron microscopy, and the influence of silane content on the mechanical properties, bonding properties and hardness of SPU adhesive was measured by universal electronic testing machine and Shore A hardness tester. The research results showed that 3-mercaptopropyl trimethoxysilane was successfully reacted to the polyurethane molecular chain, reducing the content of isocyanate group (—NCO) in the system. With the increase of silane content, the tensile strength and tensile shear properties of SPU adhesive increased, the hardness decreased, and the surface drying time was prolonged. When the silane content was 110% of the theoretical amount, the tensile strength and tensile shear strength of SPU adhesive were 0.58 MPa and 0.72 MPa, respectively, which were 7.41% and 63.64% higher than that of pure PU adhesive. The bubbles generated during curing of SPU adhesive were significantly reduced and the appearance was obviously improved.
【Keywords】one-component polyurethane adhesive; silane modification; bubble; mechanical property; tensile shear strength
Preparation of PE-g-MAH adhesive and study on its bonding properties in barrier film
Liu Yuqian1, Lyu Tongjian1,Chen Limeng2, Dong Shuhui2
(1. College of Chemistry, Liaoning University, Shenyang 110036, Liaoning, China;2. Shenyang Ketong Plastic Co., Ltd., Shenyang 101142, Liaoning, China)
【Abstract】Maleic anhydride grafted polyethylene (PE-g-MAH) was prepared by twin-screw melt extrusion. On the basis of linear low density polyethylene (LLDPE) as the matrix resin, the effects of different kinds and contents of initiators, different contents of grafted monomer maleic anhydride on the properties of PE-g-MAH prepared were discussed. At the same time, the influence of PE-g-MAH adhesive with different graft ratios, melt flow rates and number of crystal points on the bonding properties of ethylene-vinyl alcohol copolymer (EVOH) barrier film was also investigated. The grafted products were qualitatively characterized by Fourier transform infrared spectroscopy and the graft ratio of the grafted products was analyzed, the flowability was analyzed by melt flow rate test, and the bonding properties of the adhesive were analyzed by 180° peel strength test. The research results showed that when the initiator was dicumyl peroxyide (DCP) and 0.05 phr was added, and 1 phr of MAH was added at same time, the graft ratio of PE-g-MAH was 0.68%, the melt flow rate was 0.94 g·(10 min)-1, and the number of crystal points was 12, the bonding performance of the material was the best at this time. EVOH was selected as the barrier layer for bonding, when the graft ratio was 0.68%, the peel strength of PE-g-MAH reached the maximum value of 69.0 N/cm, and the bonding performance of PE-g-MAH adhesive was relatively the best.
【Keywords】maleic anhydride; adhesive; dicumyl peroxide; peel strength; ethylene-vinyl alcohol copolymer
Development and Application
Preparation and properties of reactive polyurethane hot melt adhesive for motor sealing of home appliances
Cong Helei, Fang Jun,Lang Yichao
[Kangda New Materials (Group) Co., Ltd., Shanghai 201419, China]
【Abstract】NCO-terminated prepolymer was synthesized by using polyester polyol, polyether polyol and diphenylmethane diisocyanate as raw materials.At the same time, the reactive polyurethane hot melt adhesive used for motor sealing of home appliances was prepared by using thermoplastic resin, tackifying resin and other additives. The effects of isocyanate index, polyol structure and thermoplastic resin type on their properties were investigated.The molecular structure, thermal and mechanical properties were also characterized by infrared spectroscopy, synchronous thermal analysis, and electronic universal testing machine. The research results showed that when the isocyanate index range was 1.7-2.1, the mass ratio of polyester/polyether was 2:1, and the addition amount of thermoplastic resin was 20%, the prepared reactive polyurethane hot melt adhesive had good physical properties and bonding properties to different galvanized iron and aluminum, also had excellent high and low temperature resistance, water resistance and corrosion resistance, which conformed to the operation requirements of the rapid industrial assembly line, and could be used for motor sealing of home appliances.
【Keywords】polyurethane; hot melt adhesive; fast curing; sealing; motor of home appliances
Study on high performance non-flowing prepreg
Li Zhenlin1,2, Hu Binyang2, Zhang Xueping1,2, Chen Wenqiu1,2, Fan Heping1,2
(1.Haiso Technology Co., Ltd., Wuhan 430074, Hubei, China;2. Hubei Research Institute of Chemistry, Jianghan University, Wuhan 430056, Hubei, China)
【Abstract】A kind of prepreg with excellent comprehensive performance was prepared by selecting electronic grade glass fiber cloth as the support carrier and immersing it in adhesive with high-temperature resistant epoxy resin as the main resin. The bonding strength, reflow soldering, thermal stress, dielectric resistance, dielectric withstand voltage, dielectric constant, adhesive overflowing and coefficient of thermal expansion of the prepared prepreg were systematically studied. The research results showed that the prepared high performance non-flowing prepreg had excellent properties and could meet the demand of downstream customers for the production of rigid-flex PCB.
【Keywords】non-flowing; prepreg; study
Study on characteristics of removing Ca2+from high-salt wastewater by ion exchange resin
Wu Xinsen, Yang Ye, Zhang Yang, Li Hong
(Shanghai Research Institute of Chemical Industry Co., Ltd., Shanghai 200062, China)
【Abstract】Chelating ion exchange resin was used to treat calcium ion (Ca2+) in high-salt wastewater after defluoridation of fluorochemicals. The main influencing factors and adsorption performance of the resin in the static adsorption and dynamic adsorption of Ca2+ were investigated, and the adsorption performance of the resin after multiple adsorption-regeneration was tested. The research results showed that the maximum static adsorption capacity of the resin for Ca2+ was 35.1 mg/g. When the concentration of NaCl in wastewater was 150.0 g/L, the adsorption capacity of the resin for Ca2+was only reduced by 5.2%, and the salt resistance of the resin was good. pH had little effect on the static and dynamic adsorption of the resin for Ca2+. During the dynamic adsorption process, the working adsorption capacity gradually decreased with the increase of flow rate, and the suitable flow rate should be in the range of 4-9 BV/h. When the resin was fully regenerated after saturated adsorption, the working adsorption capacity remained basically unchanged.
【Keywords】ion exchange resin; adsorption; working adsorption capacity
Special Topics and Review
High-performance thermal interface materials of thermal conductive adhesive: mechanism, status and trend
Xu Yonglun, Pang Yunsong, Ren Linlin, Sun Rong,Zeng Xiaoliang
(Shenzhen Institute of Advanced Electronic Materials, Shenzhen Institute of Advanced Technology Chinese Academy of Sciences, Shenzhen 518100, Guangdong China)
【Abstract】In this paper, the basic mechanism and model of heat transfer and bonding of thermal conductive adhesive were reviewed. The development of thermal conductivity enhancement technology of thermal conductive adhesive in recent years was analyzed and summarized. The epoxy thermal conductive adhesive and silicone thermal conductive adhesive were introduced emphatically, and the influence of new material technology on thermal conductive adhesive was discussed. Finally, the problems of thermal conductive adhesive encountered at the present stage and the possible future research directions were prospected.
【Keywords】thermal conductive adhesive; thermal interface material; coefficient of heat conductivity; thermal resistance; epoxy; silicone; self-repairing material
Current situation and future development of laminating adhesive prepared by emulsion polymerization for printing and packaging
Xia Yuzheng1, Shi Shuxian1, Ma Ji2, Chen Jianbo2
(1.College of Material Science and Engineering, Beijing University of Chemical Technology, Beijing 100029, China; 2.Shandong Xinlongyu New Material Technology Co., Ltd., Jining 272622, Shandong, China)
【Abstract】Thewaterborne laminating adhesive used in the field of printing and packaging has a history of 25 years. In the 25 years of development, from the initial development of a few companies to dozens of companies in 2006, and after more than 10 years of development, like other emulsion polymerization products, it gradually formed a monopoly situation. The paper-plastic lamination field was basically monopolized by eight companies, while waterborne lamination adhesive for plastic-plastic flexible packaging was basically monopolized by five companies. In this paper, the current situation and future development of laminating adhesive for printing and packaging were reviewed comprehensively, and effective solutions to the possible problems of crosslinking technology existing in different places of use for acrylate emulsion laminating adhesive in the field of printing and packaging in China were proposed.
【Keywords】emulsion polymerization; laminating adhesive; preparation; technical bottleneck; current situation; future development
Research progress of two-componentpolyurethane structural adhesivefor power battery in China
Deng Juan1,2, Gao Yan1,2, Liang Bin1,2, Li Jiming3, Wang Changyong3
(1.Guangzhou Mechanical Engineering Research Institute Co. Ltd., Guangzhou 510700, Guangdong, China; 2.SINOMACH Intelligence Technology Co., Ltd., Guangzhou 510700, Guangdong, China; 3.Suzhou Adhesive Technology Co., Ltd., Suzhou 215101, Jiangsu, China)
【Abstract】With the rapid development of the new energy automobile industry in China, there are more and more research and development work on two-component polyurethane structural adhesive for power battery. In this paper, the public reports, research progress and industrial technical requirements of two-component polyurethane structural adhesive for power battery in China in recent years were collected and sorted out. The main performance research included flame retardancy, thermal conductivity, aging resistance, bonding applicability to PET and removable type. Finally, the future development was prospected.
【Keywords】power battery; two-component; polyurethane; structural adhesive; patent for invention; technical requirement
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