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双语推荐：自交联

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综述了基于硅烷偶联剂室温自交联水性聚氨酯的制备方法、室温自交联固化机理及结构与性能之间的关系;硅烷偶联剂改性自交联WPU的性能、硅烷偶联剂改性特殊自交联WPU的制备、硅烷偶联剂复合交联改性WPU的制备;展望了硅烷偶联剂改性的水性聚氨酯高分子材料的发展方向和应用前景。
The progress on the self-crosslinking waterborne polyurethane at room temperature modified by organic silane coupling agent was summarized,including the preparations,self-crosslinking curing mechanism at room temperature and the relationship between the structures and properties.The performance of self-crosslinking WPU modified by silane coupling agent,the preparations of WPU modified by silane coupling, and preparations of WPU modified by composite crosslinking silane coupling were discussed.Finally,the fu-ture developments and applications of the self-crosslinking waterborne polyurethane at room temperature modi-fied by organic silane coupling agent were prospected.

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由聚氨酯(PU)乳液和聚丙烯酸酯(PA)乳液复合形成的新乳液包括物理共混聚氨酯/聚丙烯酸酯(PU/PA)复合乳液和化学共聚聚氨酯-丙烯酸酯(PUA)复合乳液,其中PUA复合乳液又可分成非交联型、合成交联型、自交联型和互穿网络型四种体系.本文较全面地综述了它们的制备方法及其特点,指出交联型PUA复合乳液既具有良好的性能又较易制造,具有广阔的工业应用前景,将成为PUA复合乳液研究开发的重点.
New emulsions formed by polyurethane (PU) emulsions and polyacrylate (PA) emulsions are classified as blend polyurethane/polyacrylate (PU/PA) composite emulsions and copolymerized polyurethane-acrylate (PUA) hybrid emulsions. PUA hybrid emulsions are divided further into four types, which are noncrossing emulsions, crossing emulsions during synthesis, crossing emulsions during film formation and interpenetrating polymer network emulsions. Preparation methods and their characteristics of PU/PA emulsion and PUA emulsions are introduced roundly. It is pointed out that the research and development of PUA hybrid emulsions would be focused on crossing PUA emulsions which are exhibiting good future of industrial applications because they can be made stably and have favorable properties.

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采用半连续种子乳液聚合方法制备了室温自交联丙烯酸树脂乳液。探讨了使用不同阴离子表面活性剂和不同引发聚合体系以及后交联剂对乳液聚合稳定性和成品革性能的影响。
A room temperature self-crosslinking acrylic resin emulsion was synthesized by semi-continuous seed emulsion polymerization method. The effects using different anionic surfactants, different initiate polymerization systems and post-crosslinking agents on emulsion stability and performance of finished leather were discussed.

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以三硫代碳酸二（α,α′-二甲基-α-乙酸）酯（BDATC）为链转移剂，以苯乙烯、马来酸酐、丙烯酸为原料，通过可逆加成-断裂链转移（RAFT）合成了双亲嵌段共聚物 PSt-b-P(St-alt-MA)-b-PAA。通过选择性溶剂 N,N-二甲基甲酰胺（DMF）诱导聚合物进行自组装，利用紫外-可见光光度仪、纳米激光粒度仪详细研究了共聚物中亲疏水嵌段长度、初始浓度、体系pH值对聚合物自组装行为的影响。通过化学交联的方法制备得到了聚合物交联胶束，利用透射电镜表征了形貌与尺寸，研究明确了其形状和尺寸的稳定性。结果表明，上述因素均会影响共聚物的自组装行为和自组装胶束的形态，经乙二胺交联得到的交联自组装胶束平均粒径为145.4nm，并具有良好的形状和尺寸稳定性。
Amphiphilic block copolymer PSt-b-P(St-alt-MA)-b-PAA was synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization using S,S′-bis(R,R′-dimethyl-α′′-acetic acid)-trithiocarbonate as RAFT agent and styrene,maleic anhydride,acrylic acid as monomers. The self-assembled micelles of PSt-b-P(St-alt-MA)-b-PAA were induced by selective solvent dimethylfomamide. The effects of block length,initial concentration and pH on the self-assembled micelles were investigated through ultra-violet and visible spectrophotometer and laser particle size analyzer. The crosslinked micelles fabricated by chemical crosslinking had stable morphology and diameter as characterized with transmission electron microscope. Block length,initial concentration and pH would affect self-assembly behavior of copolymer and morphology of self-assembled micelle. The micelles crosslinked by ethylenediamine with average particle diameter of 145.5nm had stable morphology and size.

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以丙烯酸甲酯(BA)、乙酸乙烯酯(VAC)、丙烯酸异辛酯(EHA)为主单体,丙烯酸(AA)为功能单体,丙烯酸羟乙酯(HEA)为交联单体,过硫酸铵为引发剂,合成了自交联丙烯酸酯改性无皂乳液。探讨了不同聚合条件对乳液性能的影响,确定了聚合反应的最佳合成工艺。
The self-crosslinking acrylate-modified soap-free emulsion was synthesiszed with methyl acrylate (BA), vinyl acetate (VAC) and isooctyl acrylate (EHA) as main monomer, acrylic acid (AA) as functional monomer, hydroxyethyl acrylate (HEA) as the cross-linking monomer, ammonium persulfate (APS) as initiator. The effect of polymerization conditions on properties of the emulsion was investigated and the optimal polymerization synthesis process was confirmed.

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分别合成了苯硼酸修饰的嵌段聚合物聚乙二醇-b-聚(天冬氨酸-co-天冬酰氨基苯硼酸)[PEG-b-P(Aspco-AspPBA)]和含有二硫键及多元二醇的小分子3,3''-二硫代二[1,2(S)-丙二醇](DTBPD).以DTBPD为小分子交联剂,通过二醇单元与苯硼酸之间的共价酯化作用,诱导PEG-b-P(Asp-co-AspPBA)自组装形成以苯硼酸环酯为核、PEG为壳的交联胶束.利用核磁共振氢谱和激光光散射对胶束的结构进行了表征,并分别测定了该胶束在葡萄糖和氧化-还原试剂二硫苏糖醇(DTT)刺激下的响应行为.结果表明,DTBPD可与聚合物链上的苯硼酸形成苯硼酸环酯,通过交联作用诱导聚合物形成胶束.交联度不同时,胶束对于外界刺激(葡萄糖和DTT的响应行为也不同:随着DTT和葡萄糖浓度的增加,交联度高的胶束只发生响应性溶胀,交联度低的胶束则先溶胀,之后溶胀程度较大的部分胶束则发生解体,导致胶束的平均粒径减小.
Phenylboronic acid modified polymer poly(ethylene glycol)-b-poly(aspartic acid-co-aspartamido-phenylboronic acid)[PEG-b-P(Asp-co-AspPBA)] as well as a cross-linker 3,3’-dithiobis[1,2(S)-propane-diol](DTBPD) which contained disulfide bond and dual-diol groups was successfully synthesized. PEG-b-P(Asp-co-AspPBA) could be mildly cross-linked by DTBPD based on the reaction of PBA and the dual-diol groups, leading to the formation of a novel dual-responsive micelle with boronic ester core and PEG shell. The structure, morphology, and the glucose / redox dual-responsive behavior of the micelles were systematically in-vestigated by nuclear magnetic resonance(NMR) spectrum and dynamic laser light scattering(DLS). It was demonstrated that the ratio of diol to PBA(D : B) had influence on the dual-responsive behavior of the mi-celles. At higher ratio of D : B, only responsive swelling of micelles was observed. While for the micelles with lower ratio of D : B, larger degree of swelling

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以共轭亚油酸(Conjugated linoleic acid,CLA)为构造pH非敏感型脂肪酸囊泡(Fatty acid vesicle,FAV)的分子砌块,通过碱异构化法从亚油酸半合成CLA,然后采用pH刺激响应自组装法获得CLA的不饱和脂肪酸囊泡(Ufasome),采用紫外辐照诱导方式对CLA-ufasome实施囊泡内化学绑定,获得一种新的pH非敏感型FAV.通过酸碱滴定和表面张力实验确定CLA-ufasome形成的适宜pH范围和浓度,利用透射电子显微镜(TEM)表征了自交联CLA的FAV的形貌,并通过动态光散射(DLS)法测定了自交联CLA的FAV的稳定性.结果表明,以CLA为分子砌块,当浓度为3 mmol/L时在pH=8.6条件下构建CLA-ufasome,紫外辐照2.5 h后得到粒径为10~20 nm,壁厚为2.0 nm的自交联CLA的FAV,并具有pH非敏感的特性.以抗癌药物五氟尿嘧啶为目标包覆药物,体外释放实验结果表明,自交联CLA的FAV对五氟尿嘧啶具有良好的缓释效果.
Conjugated linoleic acid( CLA) was employed as a molecular building block to construct a novel pH-insensitive fatty acid vesicle(FAV). First, CLA was semi-synthesized from linoleic acid through alkali isomerization. Subsequently, the ufasome(unsaturated fatty acid liposome) of CLA was self-assembled from the CLA molecules together with the CLA ions in response to pH, and a novel pH-insensitive FAV, the self-crosslinked-CLA FAV, was prepared by chemical tethering the CLA-ufasome through UV irradiation. The sui-table pH ranges and the CLA concentrations were determined by acid-base titration and surface tension mea-surement. The morphology of the self-crosslinked-CLA FAV was imaged by transmission electro microscopy ( TEM) and the pH-insensitive characteristic of the self-crosslinked-CLA FAV was tested by dynamic light scattering ( DLS ) . The experimental results indicated that the self-crosslinked-CLA FAV with diameter of 10-20 nm and wall thickness of 2.0 nm was obtained through a two

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以三羟甲基丙烷三甲基丙烯酸酯（ TMPTMA ）为内交联单体,苯乙烯（ St ）、甲基丙烯酸甲酯（ MMA）、丙烯酸丁酯（ BA）和甲基丙烯酸（ MAA）为共聚单体,采用半连续核壳乳液聚合工艺合成了自交联聚丙烯酸酯乳液（ T-PAE）。考查了TMPTMA添加量与添加方式对乳液聚合稳定性以及涂膜性能的影响。研究发现：随着TMPTMA含量的增加,T-PAE乳液聚合的稳定性降低,聚合凝胶率增大,乳胶粒的平均粒径下降；涂膜的耐介质性能和交联密度相应提高,合适的TMPTMA加入量为总单体质量的0．5%~1．0%。
The crosslinked polyacrylate latexes( T-PAE) with core-shell structure were synthesized by semi-batch core-shell emulsion polymerization process with trimethylol propane trimethacrylate ( TMPTMA ) as a crosslinker, methyl acrylate( MMA) ,styrene( ST) ,butyl acrylate( BA) and methacrylic acid( MAA) as co-monomers. The effects of the contents and added methods of TMPTMA on the emulsion and film properties were investigated. The results indicated that the polymerization stability and particle sizes of T-PAE decreased with the amount of TMPTMA in-creased,while the water-or alcohol-resistance properties of cured film improved due to increasing of the crosslinked degrees of T-PAE film,the optimal TMPTMA dosage is 0. 5~1. 0wt%.

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采用预乳化半连续乳液聚合的方法，从6种不同的自交联单体中，筛选出乳液性能良好，涂料印花织物焙烘温度最低、无甲醛释放的自交联单体HA。确定了最佳印花工艺为：预烘温度80℃，时间3 min；焙烘温度110℃，时间3 min。测试结果表明，印花织物耐干、湿摩擦色牢度和耐皂洗色牢度与市售的涂料印花粘合剂等级相当。透射电镜（TEM）表明乳胶粒单分散性良好，绝大多数呈球状。
The emulsion of styrene, butyl-acrylic and 2-ethylhexyl acrylate was prepared by pre-emulsification and semi-continuous polymerization method. From six different self-crosslinking monomer, the formaldehyde-free cross-linking monomer HA was singled out on condition that the emulsion performance was better and the curing temperature of the pigment printing fabric was the lowest. Then, the optimum printing process was established as following that the temperature and time of the procuring were 80℃ and 3 min,and the temperature and time of the curing were 110℃ and 3 min. Compared with the commercially available pigment printing binder, to dry and wet rubbing fastness and the washing fastness of the printed fabrics were comparative. Finally, transmission electron microscopy indicated that the emulsion particles were mono-dispersed and mostly spherical in shape.

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要: 以超临界CO2为反应介质,制备了三氟氯乙烯(CTFE)-乙酸乙烯酯(VAc)-马来酸酐(MAH)共聚物[P(CTFE-VAc-MAH)].考察了单体配比对聚合反应及聚合物结构、性能的影响,研究了聚合物的自乳化性能及交联反应.结果表明:在m(VAc)/m(CTFE)为6∶14的聚合体系中,增加MAH单体的比例,聚合物颗粒逐渐减小,产物中的氟含量逐渐降低;通过溶液法可使P(CTFE-VAc-MAH)共聚物形成自乳化乳液,乳胶粒的粒径随着聚合物中MAH比例的增大而变小;此共聚物在一定条件下可与多元醇或多元胺类发生交联反应.
@@@@The chlorotrifluoroethylene (CTFE)-vinyl acetate (VAc)-maleic anhydride (MAH) copolymer [P(CTFE-VAc-MAH)] was produced in supercritical carbon dioxide. The effect of monomer ratio on the polymerization and the structure and properties of the polymer was investigated, and the self-emulsifying property and the cross-linking reaction of the polymer were studied. The results show that the polymer particles become smaller and the fluorine content in the polymer gets lower gradually with increasing the amount of MAH monomer when the mass ratio of VAc to CTFE is 6∶14. P(CTFE-VAc-MAH) self-emulsifying latex can be obtained by solution method, and the sizes of the latex particles become smaller with the increase in the content of MAH in the polymer. The polymer can take place the cross-linking reaction with polyamine and polyol on certain conditions.

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