异构十醇聚氧乙烯醚与阴离子表面活性剂复配体系的性能研究

对异构十醇聚氧乙烯醚(IC_(10)EO_n)、十二烷基苯磺酸钠(LAS)和脂肪醇聚氧乙烯(2)醚硫酸钠(C_(12~14)E_2S)的水溶性进行分析,研究了LAS和C_(12~14)E_2S对异构十醇聚氧乙烯(8)醚(IC_(10)EO_8)浊点的影响,同时考察了IC_(10)EO_8与LAS和C_(12~14)E_2S复配体系的润湿力、泡沫性能、去污力等。结果表明,在25℃下,当IC_(10)EO_n的EO加合数为3,8和9时可与水以任意比例互溶,不会形成凝胶;在IC_(10)EO_8与LAS和C_(12~14)E_2S的复配体系中,当LAS和C_(12~14)E_2S的质量分数大于0.6%时,浊点迅速上升;IC_(10)EO_8与LAS和C_(12~14)E_2S的质量比在3∶1~1∶3范围内,复配体系的润湿性能优于单一表面活性剂,当IC_(10)EO_8与LAS和C_(12~14)E_2S的质量比为1∶1时,润湿性能最佳;IC_(10)EO_8的泡沫性能较差,随着阴离子表面活性剂的含量增加,复配体系起泡力逐渐增强,泡沫稳定性呈不规则变化;加入一定量的阴离子表面活性剂可提高IC_(10)EO_8的去污力。     

椰油酰胺丙基甜菜碱与脂肪醇聚氧乙烯醚羧酸钠复配性能研究

考察椰油酰胺丙基甜菜碱(CAB-35)与脂肪醇聚氧乙烯醚羧酸钠(AEC-9)复配体系的稳定性、表面性能、泡沫性能和润湿性能。结果表明,复配体系稳定性良好,在28%质量浓度范围内为均匀透明的溶液;复配体系具有一定的协同作用,在m(CAB-35)∶m(AEC-9)=8∶2时,临界胶束浓度为最小值52.95 mg/L,最小表面张力26.4 mN/m,表面的饱和吸附量达到最大(7.19×10~(-6)mol/m~2),极性头基所占的截面积最小(0.23×10~(-18)m~2)。在此比例下,复配体系的表面活性最高,同时发泡能力、稳泡性和润湿性也达到最优值。     

椰油酰胺丙基甜菜碱与脂肪醇聚氧乙烯醚羧酸钠复配性能研究

考察椰油酰胺丙基甜菜碱(CAB-35)与脂肪醇聚氧乙烯醚羧酸钠(AEC-9)复配体系的稳定性、表面性能、泡沫性能和润湿性能。结果表明,复配体系稳定性良好,在28%质量浓度范围内为均匀透明的溶液;复配体系具有一定的协同作用,在m(CAB-35)∶m(AEC-9)=8∶2时,临界胶束浓度为最小值52.95 mg/L,最小表面张力26.4 mN/m,表面的饱和吸附量达到最大(7.19×10^(-6)mol/m(-6)mol/m²),极性头基所占的截面积最小(0.23×102),极性头基所占的截面积最小(0.23×10^(-18)m(-18)m²)。在此比例下,复配体系的表面活性最高,同时发泡能力、稳泡性和润湿性也达到最优值。     

脂肪醇聚氧乙烯醚羧酸钠与十二烷基三甲基氯化铵的复配性能

研究了脂肪醇聚氧乙烯醚羧酸钠(AEC-9)与十二烷基三甲基氯化铵(1231)复配体系的表面性能、稳定性、泡沫性能和润湿性能.结果表明:复配体系具有很好的稳定性,在形成胶束的能力及降低表面张力的能力方面相对单一组分均有显著提高;当n(AEC-9):n(1231)=1:1时协同增效作用最为明显,其γcmc(27.0 Mn/m)和cmc(0.140 mmol/L)要明显低于单一组分AEC-9(35.5 Mn/m,0.196 mmol/L)和1231(37.0 Mn/m,8.77 mmol/L),起泡力(425 Ml)、稳泡性(0.99)和润湿性(1.2 min)均显著优于单一组分AEC-9(355 Ml,0.89,17.2 min)和1231(365 Ml,0.90,21.0 min).     

脂肪醇聚氧乙烯醚磷酸酯的合成

以脂肪醇聚氧乙烯醚(AEO-3)为原料,P2O5为磷酸化试剂,经酯化、水解合成脂肪醇聚氧乙烯醚磷酸酯.考察了P2O5加入方式、原料配比、酯化时间、酯化温度对反应的影响.     

脂肪醇聚氧乙烯醚磷酸酯三乙醇胺盐的研制及其应用

以脂肪醇和环氧乙烷为原料,五氧化二磷为酯化剂,三乙醇胺为中和剂,合成了脂肪醇聚氧乙烯醚磷酸酯三乙醇胺盐,对其合成工艺及其复配油剂在腈纶上的应用进行了研究。结果表明,最佳合成工艺条件为:环氧乙烷与脂肪醇的摩尔比为2．0,脂肪醇聚氧乙烯醚与五氧化二磷的摩尔比为3．8,五氧化二磷投料时间1．5 h,酯化温度70℃,酯化反应时间3．0 h,三乙醇胺的加入量是脂肪醇聚氧乙烯醚磷酸酯的0．73-0．76 倍。用酯肪醇聚氧乙烯醚磷酸酯三乙醇胺盐为单体复配的油剂,其在腈纶中的应用情况与进口日本油剂相当。     

烯丙基脂肪醇聚氧乙烯醚的合成及应用研究

以脂肪醇聚氧乙烯醚、氢氧化钠以及烯丙基氯为主要原料,合成了烯丙基脂肪醇聚氧乙烯醚。在优化的反应工艺条件下,产品总收率可达95%(以脂肪醇聚氧乙烯醚为基准计算)。使用红外光谱对中间体烯丙基脂肪醇聚氧乙烯醚进行了结构鉴定,并测试了产品和原料的表面(界面)性能(γcmc,πcmc,cmc,πcmc,pC20,Γm,Am)以及应用性能(润湿、乳化、泡沫)。结果表明,产品表面性能变化不大,并且具有低泡及润湿性能优良的特点。     

窄分布脂肪醇聚氧乙烯醚硫酸钠的性能研究

分别对工业化的常规脂肪醇聚氧乙烯醚(AEO_2)和窄分布AEO_2进行气相色谱分析,并对以2种AEO_2为原料生产的脂肪醇聚氧乙烯醚硫酸钠(AES)的表面活性、泡沫性能、乳化性能、润湿性能以及倾点等进行研究。通过对2种AEO_2的气相色谱分析发现,窄分布AEO_2中游离脂肪醇含量更低,EO加合数为1~4的组分含量更高。将2种AES产品的性能进行对比后发现,窄分布AES在倾点、盐增稠能力、泡沫性能、润湿力等方面较常规AES具有一定的优势。     

脂肪醇聚氧乙烯醚甲基丙烯酸酯的合成

以脂肪醇聚氧乙烯醚和甲基丙烯酸为原料,混合催化剂T为催化剂,对苯二酚为阻聚剂,通过酯化反应直接合成了脂肪醇聚氧乙烯醚甲基丙烯酸酯。探讨了催化剂种类、催化剂用量、反应物配比、反应时间和反应温度对酯化反应的影响。结果表明,适宜的合成工艺条件为:n(脂肪醇聚氧乙烯醚)∶n(甲基丙烯酸)=1∶1.8,混合催化剂T的用量为脂肪醇聚氧乙烯醚量的2%,用甲苯作带水剂,反应温度150℃,反应时间5 h,阻聚剂的用量为丙烯酸量的0.5%。在此条件下,酯化率可达99.4%。     

长链脂肪醇聚氧乙烯醚丙酸盐的合成与性能

以脂肪醇聚氧乙烯醚、丙烯酸甲酯、氢氧化钠为主要原料,经过加成、皂化反应,合成脂肪醇醚丙酸盐(AEP)。采用IR、质谱对产物结构进行了表征,证明所得产物即为目标产物。测定了AEP的相关性能,结果表明,C12AEP在25℃时,CMC和γCMC分别为0.236 mmol/L和26.63 mN/m;采用稳态荧光法以芘(Py)为荧光探针,测定C12AEP的胶束栅栏层的微极性,较一般表面活性剂小;AEP与甜菜碱(B)复配体系界面张力受硬度、盐度及复配比例的影响较大,C18AEP与甜菜碱(B)复配体系可达到3.98×10-3mN/m的超低界面张力,可适用于石油的三次开采。     

Effect of dihydroxydiphenyl ether on poly(ether ether ketone)

A series of modified poly(ether ether ketone) (PEEK) polymers were synthesized by introduction of addition ether groups from dihydroxydiphenyl ether (DHDE) into the PEEK structure. The inherent viscosity of the DHDE-modified PEEK increased with reaction time at 320 °C. DSC thermograms showed the melting points of the obtained PEEK decreased with the increase of the DHDE content in the backbone. The degradation temperature (T_d) was slightly decreased by the introduction of DHDE. The crystallinity as measured via the X-ray diffraction (XRD) increases with the introduction of DHDE into the modified PEEK. The crystalline structure was identified as an orthorhombic structure with lattice constants a = 7.72 Å, b = 5.86 Å, and c = 10.24 Å. Due to the glass transition temperature (T_g) and the melting temperature (T_m) decreasing with the increase of the DHDE content in the reaction system. the processability of the resultant PEEK could be improved through this DHDE modification.     

Fine poly(ether ether ketone) powders

The physical form of polymers is often important for carrying out subsequent processing operations. For example, fine powders are desirable for molding and sintering compounds because they consolidate to produce void free components. The objective of this work is to prepare fine polymeric particulates suitable for processing into fiber reinforced polymer matrix composites. Micron size particles of poly(ether ether ketone) (PEEK) were prepared by rapidly quenching solutions of these materials. PEEK pellets were dissolved at temperatures near the PEEK melting point in a mixture of terphenyls and quaterphenyls; then the solution was quenched to a temperature between the T_g and T_m (≈ 225°C) by adding a room temperature eutectic mixture of diphenyl ether and biphenyl. A supersaturated, metastable solution of PEEK resulted, causing rapid nucleation. Fine PEEK particles rapidly crystallized from this solution. The average particle size was measured using transmission electron microscopy, atomic force microscopy, and by light scattering of aqueous suspensions which had been fractionated by centrifugation. The average particle diameter was about 0.6 μm. Three dimensional photomicrographs obtained via atomic force microscopy showed some aggregates in the suspensions. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 63: 1571–1578, 1997     

Synthesis and properties of thio‐containing poly(ether ether ketone)s

A series of thio‐containing poly(ether ether ketone) (PEESK) polymers was synthesized by the introduction of thio groups from 4,4′ thiodiphenol (TDP) into the poly(ether ether ketone) (PEEK) structure via reaction between the phenol and aromatic fluoride groups. The effect of the thio groups on the properties of the PEESK materials was investigated. Differential scanning calorimetry (DSC) analysis and X‐ray diffraction (XRD) patterns show a depression in the crystallinity of the PEESKs with incorporation of the content of thio groups in the backbones. The crystalline structure was identified as an orthorhombic structure with lattice constants of a = 7.52 Å, b = 5.86 Å and c = 10.24 Å for all crystallizable PEESKs. The crystalline structures of the thio‐containing PEEK polymers were the same as that of the neat PEEK, which means the thio‐containing block in the whole thio‐containing PEEK molecule is almost excluded from the crystalline structure and the crystals are completely formed by ‘non‐thio’ blocks only. Due to the glass transition temperature (T_g) and melting temperature (T_m) depression with increase in the TDP content in the reaction system, the processability of the resultant thio‐containing PEEKs could be effectively improved. Copyright © 2004 Society of Chemical Industry     

两种双取代苯并冠醚的合成

以邻苯二酚为原料,采用不同的方法合成了两种双取代苯并冠醚,并进行了结构表征,确认其组成。     

Miscibility and crystallization behavior of poly(ether ether ketone ketone)/poly(ether imide) blends

The miscibility and crystallization behavior of poly(ether ether ketone ketone) (PEEKK)/poly(ether imide) (PEI) blends prepared by melt‐mixing were investigated by differential scanning calorimetry. The blends showed a single glass transition temperature, which increased with increasing PEI content, indicating that PEEKK and PEI are completely miscible in the amorphous phase over the studied composition range (weight ratio: 90/10–60/40). The cold crystallization of PEEKK blended with PEI was retarded by the presence of PEI, as is apparent from the increase of the cold crystallization temperature and decrease of the normalized crystallinity for the samples anealed at 300°C with increasing PEI content. Although the depression of the apparent melting temperature of PEEKK blended with PEI was observed, there was no evidence of depression in the equilibrium melting temperature. The analysis of the isothermal crystallization at 313–321°C from the melt of PEEKK/PEI (100/0, 90/10, and 80/20) blends suggested that the retardation of crystallization of PEEKK is caused by the increase of the crystal surface free energy in addition to the decrease of the mobility by blending PEI with a high glass transition temperature. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 769–775, 2001     

聚醚醚酮表面壳聚糖的固定

通过紫外光接枝和湿化学法连用在聚醚醚酮 （PEEK）表面固定上具有抑菌杀菌作用的壳聚糖。结果表明,相比未改性的PEEK表面,改性后材料表面亲水性提高;通过扫描电子显微镜和X射线光电子能谱分析证明壳聚糖成功接枝在了PEEK薄膜表面;随着壳聚糖浓度的提高,材料表面的壳聚糖接枝率增加。     

Spherulitic growth kinetics in miscible blends of poly(ether ether ketone) and poly(ether imide)

Growths of poly(ether ether ketone) (PEEK) spherulites from both pure melt and its miscible blends with poly(ether imide) (PEI) have been studied by polarized optical microscopy. The nucleation density of PEEK spherulites was depressed upon blending with PEI, which can be attributed to the reduction in degree of supercooling arising from equilibrium melting point depression. A modified Lauritzen-Hoffman (L-H) theory was adopted to analyze the growth kinetics. Regime III-II transition was observed with the transition temperature decreasing with increasing PEI composition. Assuming free rotations of the virtual bonds in PEEK molecule, the side surface free energy of 12.0 erg/cm² was calculated from the characteristic ratio. The fold surface free energy of 188 erg/cm² and work of chain folding of 12.3 kcal/mol were then obtained from the modified L-H analysis.     

聚苯酯对聚醚醚酮结晶行为的影响

用模压法制备了聚苯酯(Ekonol)／聚醚醚酮(PEEK)复合材料，通过X射线衍射(XRD)、差示扫描量热分析(DSC)考察了PEEK的结晶行为，并测定了复合材料的熔点、结晶温度和玻璃化转变温度。结果表明：Ekonol含量的大小对PEEK的结晶行为产生了直接影响，PEEK的相对结晶度随着Ekonol含量的增加而提高；Ekonol含量小于30％时，对复合材料的熔点、结晶温度和玻璃化转变温度影响不大，但含量大于30％时，材料的结晶温度、熔融温度下降，玻璃化转变温度提高。     

聚醚砜/磺化聚醚醚酮共混膜的制备和性能

采用流延法制备了聚醚砜(PES)含量不同的PES/磺化聚醚醚酮(SPEEK)共混膜。PES与SPEEK具有良好的相容性。所制备PES/SPEEK共混膜的含水率、溶胀度和甲醇透过系数均随PES含量的增加而降低。虽然共混膜的质子传导性能有所降低.但阻醇性能和溶胀性能提高,这说明PES/SPEEK共混膜是一种很好的直接甲醇燃料电池用固体高分子电解质膜材料。     

Synthesis and characterization of poly(ether amide ether ketone)/poly(ether ketone ketone) copolymers

A new monomer, N,N′‐bis(4‐phenoxybenzoyl)‐m‐phenylenediamine (BPPD), was prepared by condensation of m‐phenylenediamine with 4‐phenoxybenzoyl chloride in N,N‐dimethylacetamide (DMAc). A series of novel poly(ether amide ether ketone) (PEAEK)/poly(ether ketone ketone) (PEKK) copolymers were synthesized by the electrophilic Friedel‐Crafts solution copolycondensation of terephthaloyl chloride (TPC) with a mixture of diphenyl ether (DPE) and BPPD, over a wide range of DPE/BPPD molar ratios, in the presence of anhydrous AlCl₃ and N‐methylpyrrolidone (NMP) in 1,2‐dichloroethane (DCE). The influence of reaction conditions on the preparation of copolymers was examined. The copolymers obtained were characterized by different physicochemical techniques. The copolymers with 10–25 mol % BPPD were semicrystalline and had remarkably increased T_gs over commercially available PEEK and PEKK due to the incorporation of amide linkages in the main chains. The copolymers III and IV with 20–25 mol % BPPD had not only high T_gs of 184–188°C, but also moderate T_ms of 323–344°C, having good potential for the melt processing. The copolymers III and IV had tensile strengths of 103.7–105.3 MPa, Young's moduli of 3.04–3.11 GPa, and elongations at break of 8–9% and exhibited outstanding thermal stability and good resistance to organic solvents. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011