2,2’-双[4-(4-氨基苯氧基)苯基]丙烷的制备方法

介绍了以2,2’-双(4-羟基苯基)丙烷、对氯硝基苯,碱金属碳酸盐或碱金属氢氧化物为原料,在合适的溶剂中合成2,2’-双[4-(4-硝基苯氧基)苯基]丙烷,再经不同还原方法制备2,2’-双[4-(4-氨基苯氧基)苯基]丙烷。并从反应工艺条件、产品收率、产物纯度、是否适合规模化生产等方面阐述了制备2,2’-双[4-(4-氨基苯氧基)苯基]丙烷方法的优缺点。通过比较、分析指出了2,2’-双[4-(4-氨基苯氧基)苯基]丙烷的研究和发展方向。     

2,2-二(3-氨基-4-羟基苯基)六氟丙烷的合成

以2,2-二(4-羟基苯基)六氟丙烷为原料,分别经硝化和还原反应合成出2,2-二(3-氨基-4-羟基苯基)六氟丙烷。并在实验室小试成功后,进行工厂中试研究,以确定中试的各个工艺参数。结果表明,对于第1步硝化反应,以乙醇做溶剂,用量为n(乙醇)/n〔2,2-二(4-羟基苯基)六氟丙烷〕=4,n(稀硝酸)/n〔2,2-二(4-羟基苯基)六氟丙烷〕=2.15,反应温度为60℃,反应时间为6 h的条件下,合成2,2-二(3-硝基-4-羟基苯基)六氟丙烷的产率达到最高值96%。对于第2步还原反应,采用自制FeCl3/活性炭为催化剂,乙醇做溶剂,n(水合肼)/n〔2,2-二(3-硝基-4-羟基苯基)六氟丙烷〕=0.2,m(FeCl3/活性炭)/m〔2,2-二(3-硝基4-羟基苯基)六氟丙烷〕=0.05,反应温度为85℃,反应时间为10 h的条件下,合成2,2-二(3-氨基-4-羟基苯基)六氟丙烷的产率达到最高值92%。该工艺条件在工厂已进行了中试研究,确定了工业实验的各个工艺参数和工艺条件。     

Cu改性BN/聚苯腈复合材料的制备及其导热性能研究

以2,2-二(4-羟基苯基)丙烷和4-硝基邻苯二甲腈为原料合成了2,2-双[4-(3,4-二氰基苯氧基)苯基]丙烷(BDPP)。将BDPP作为基体,以Cu改性后的氮化硼(BN)为填料,制备出了Cu改性BN/聚苯腈导热复合材料。结果表明:制备出纯度较高的BDPP单体和双酚A型聚苯腈树脂;Cu成功沉积在BN表面,改善了BN表面的可润湿性;添加Cu改性BN后,BN/聚苯腈复合材料的热导率明显提高,从0.24 W/(m·K)增至0.85 W/(m·K)。     

2,2-二(3-氨基-4-羟基苯基)六氟丙烷的合成研究

以2,2-二(3-硝基-4-羟基苯基)六氟丙烷为主要原料,水合肼作还原剂,乙醇作做溶剂,钯碳做催化剂,合成了2,2-二(3-氨基-4-羟基苯基)六氟丙烷。通过正交实验确定了其最佳合成条件:反应温度为80℃,n(2,2-二(3-硝基-4-羟基苯基)六氟丙烷)∶n(水合肼)=0.25∶1,m(钯碳)∶m(2,2-二(3-硝基-4-羟基苯基)六氟丙烷)=0.015∶1,m(乙醇)∶m(2,2-二(3-硝基-4-羟基苯基)六氟丙烷)=4∶1,反应时间12 h,产品收率达到92.2%。     

2，2-二(3-氨基-4-羟基苯基)六氟丙烷的合成、用途及发展前景

介绍了2,2-二(3-氨基-4-羟基苯基)六氟丙烷的合成方法,叙述了2,2-二(3-氨基-4-羟基苯基)六氟丙烷作为合成含氟聚酰亚胺单体的应用和一些其它用途.另外还阐述了其发展前景.     

(2,2-双二茂铁基丙烷)-6,6′-二甲酸的合成与表征

用2,2-双二茂铁基丙烷与邻氯苯甲酰氯在AlCl3催化下合成了6,6′-二(邻氯苯甲酰基)双二茂铁基丙烷,然后在叔丁醇钾的存在下解离成相应的(2,2-双二茂铁基丙烷)-6,6′-二甲酸。利用元素分析、红外光谱和核磁共振氢谱对合成的化合物进行了表征。     

含氟环氧树脂

按下列步骤先合成了2,2-双-(对-环氧丙氧基苯基)-六氟丙烷(Ⅱ)(白色晶体,熔点96～98°)。再和2,2-双-(对-羟苯基)-六氟丙烷(Ⅰ)作用即可获得分     

2,2-二(3,5-二氨基- 4-羟基苯基)丙烷的合成

2,2-二(3,5-二氨基-4-羟基苯基)丙烷是一种新型膨胀型阻燃剂和合成N-P系膨胀型阻燃剂的中间体。研究了Fe-A l/C催化水合肼还原2,2-二(4-羟基-3,5-二硝基苯基)丙烷合成2,2-二(3,5-二氨基-4-羟基苯基)丙烷的反应条件。结果表明:对20 mmol的反应物,Fe-A l/C催化剂的用量为0.6 g,反应温度为75℃,反应时间为5 h,物料比n〔2,2-二(4-羟基-3,5-二硝基苯基)丙烷〕∶n(水合肼)=1∶12时,还原产率为93.75%,w〔2,2-二(3,5-二氨基-4-羟基苯基)丙烷〕=96.5%(HPLC),Fe-A l/C催化剂可以重复使用7次。产物经元素分析、红外光谱、核磁共振和质谱分析确证。     

双酚A型二胺和二酐合成可溶性聚酰亚胺的研究

采用2,2-双[4-(4-氨基苯氧基)苯基]丙烷(BAPP)和2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐(BPADA)为单体,N,N-二甲基甲酰胺(DMF)为溶剂,通过常规的两步法,并分别经热亚胺化和化学亚胺化过程合成了双酚A型聚酰亚胺(PI).用FTIR、DSC、TGA等对聚合物的结构和性能进行了表征.F...     

2,2-二甲基环丙烷甲酸的合成与拆分

S-( )-2,2-二甲基环丙烷甲酸是合成西司他丁(一种肾脱氢二肽酶抑制剂)的关键中间体,今设计了一条新的2,2-二甲基环丙烷甲酸合成路线并改进了拆分工艺,它是以异戊烯酸为原料,经酸的酯化、烯键的环丙烷化、酯水解制得2,2-二甲基环丙烷甲酸,收率为44．1％。其中,环丙烷化反应用锌粉／氯化亚铜-乙酰氯作为催化剂,二溴甲烷作为环丙烷化试剂,这样可以在温和的条件下进行反应,降低成本。此外用L-肉碱草酸盐作为手性拆分试剂,经酰化、成盐、部分结晶、水解得到S-( )-2,2-二甲基环丙烷甲酸．收率为16．7％,手性纯度大于95％．此路线工艺简单、环境友好、成本较低,易于工业化。     

双组分醇溶型聚氨酯胶粘剂的研制

通过分子结构设计,利用异佛尔酮二异氰酸酯（IPDI）预聚物与异佛尔酮二胺（IPDA）扩链反应,合成端氨基聚氨酯主胶,再以环氧树脂为固化剂、乙醇为溶剂,成功制备了双组分醇溶型聚氨酯胶粘剂。研究了第二层膜复膜时间对固化后包装膜形貌的影响,得出在第二层复膜时要充分挥发溶剂。通过测定不同配方的固化时间,发现预聚物分子链越长,固化越慢。同时,比较了自制样品与通用聚氨酯胶粘剂产品的粘度与剥离强度,证实了自制双组分醇溶型聚氨酯胶粘剂的性能与市场上的产品相当,且可通过加大固化剂的添加比例来提高力学性能。     

硬段含量对聚氨酯和聚氨酯脲氢键化程度的影响

以PPG600,PPG2000,甲苯二异氰酸酯(TDI)和1,4-丁二醇(1,4-BD)为原料合成了聚氨酯(PU),通过改变PPG600,PPG2000配比调节产品硬段含量;以PPG2000,TDI和异佛尔酮二胺(IPDA)为原料合成了聚氨酯脲(PUU),通过调节TDI与IPDA在体系中的比例调节产品硬段含量。利用FT-IR,DSC,旋转黏度计研究了硬段含量对聚醚型PU和PUU的微观结构及黏度的影响。结果表明,随硬段含量提高,PU和PUU的氢键化程度均提高,PU较多地形成不完善的氢键,而PUU倾向于形成完善有序的氢键结构。此外随硬段含量增大,PU和PUU的黏度增大,PU软段的玻璃化转变温度升高。     

Preparation and property of waterborne UV‐curable chain‐extended polyurethane surface sizing agent: Strengthening and waterproofing mechanism for cellulose fiber paper

Waterborne UV‐curable polyurethane (UWPU) dispersions with different hydrophilicity and functionalities were prepared by varying the content of dimethylol butanoic acid (DMBA) and pentaerythritol triacrylate (PETA). And linear and cyclic chain extenders with different functionalities were also incorporated into the UWPU backbone, including isophorone diamine (IPDA), diethylene triamine (DETA), and ethylene diamine (EDA). Effects of DMBA content, PETA content, photoinitiator content, UV curing time, chain extender on the properties of UWPU dispersions and films, as well as the properties of the unsized and sized paper were investigated. The water resistance and mechanical properties of sized paper were greatly relied on the particle size, the molecular weight, the croslinking density, and penetrability of UWPU. UWPU dispersion chain extended with IPDA (IPDA‐UWPU) displayed smaller particle size than that of UWPU. The paper sized with IPDA‐UWPU was endowed with best water resistance, tensile strength, folding strength and surface strength. XPS depth analysis revealed that IPDA‐UWPU exhibited better penetrability into the paper substrate than UWPU. SEM and AFM demonstrated that the smoothness of sized paper was improved, and the bond strength between fibers was enhanced. The obtained UWPU could be directly used as an effective and fast drying surface sizing agent for cellulose fiber paper. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42354.     

Preparation and characterization of innovative cellulose diacetate/epoxy resin blends modified by isophorone diamine

Cellulose diacetate (CA)/epoxy resin (EP) blends with excellent mechanical performance were prepared with simple blending followed by curing with isophorone diamine (IPDA). The reaction between the amino groups of IPDA and epoxide groups of EP was confirmed by Fourier transform infrared spectroscopy. Scanning electron microscopy revealed that the cured EP particles gradually became larger and closer to each other to form semi‐interpenetrating polymer networks in the CA matrix; this contributed to the improved mechanical properties of the CA/EP blends. Dynamic rheological experiments indicated that the CA/EP blends with semi‐interpenetrating polymer networks retained processability. After the introduction of a low content (5–10 phr) of IPDA, the mechanical properties of the CA/EP blends were significantly enhanced. With the addition of 20–30‐phr IPDA, the CA/EP blend exhibited a tensile strength of 77 MPa, a flex strength of 65 MPa, a flex modulus of 2.6 GPa, and a hardness of 94 HD; these values were much higher than those of the pristine CA/EP binary blend. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44151.     

固体推进剂用异佛尔酮二异氰酸酯的生产技术

比较了异佛尔酮二异氰酸酯（IPDI）的生产方法和经济性,传统光气法收率高,但毒性大,非光气法特别是DMC法反应条件温和,环境污染小,虽比光气法生产成本增加了5.45%,但仍然具有广泛的工业化应用前景。     

不同二胺类后扩链剂对水性聚氨酯性能的影响

以异佛尔酮二异氰酸酯、聚四氢呋喃醚、聚碳酸己二醇酯和二羟甲基丙酸等为主要原料合成了水性聚氨酯(WPU),研究了乙二胺、二乙烯三胺和异佛尔酮二胺分别作为后扩链剂对乳液稳定性和成膜物性的影响。结果表明,以异佛尔酮二胺后扩链制备的WPU综合性能较好;随着异佛尔酮二胺用量的增加,WPU乳液稳定性提高,胶膜的耐水和耐溶剂性能提高,力学性能改善,但扩链比例过高,不利于WPU综合性能的改善,在本实验条件下,适宜的扩链比例为75%。     

环氧树脂和环氧/环硫树脂与胺的固化反应动力学

采用非等温DSC法对低黏度体系CY184/IPDA环氧树脂体系及对CY184/ES184/IPDA环氧/环硫树脂体系的固化反应动力学进行了研究。用高级等转化率Vyazovkin积分法求取活化能E_a,通过Málek法确定了固化反应机理函数和动力学参数,得到固化反应动力学方程。结果表明:CY184/IPDA环氧树脂体系的平均活化能为47.04 kJ·mol^-1;CY184/ES184/IPDA环氧/环硫树脂体系的活化能为48.97 kJ·mol^-1。两种体系的模型拟合曲线与实验得到的DSC曲线吻合得较好,均符合esták-Berggren(m,n)模型。     

C36二聚酸改性环氧树脂涂料的制备与性能研究

C36二聚酸与双酚A型环氧树脂(DGEBA)反应制备出分子结构中含有疏水烷烃链的端环氧基预聚物(DAMPE),用傅里叶红外光谱仪(FT-IR)对其结构进行了表征。以不同用量的DAMPE与环氧树脂混合后用等物质的量的改性异佛尔酮二胺固化剂(IPDA)固化,制得了不同C36二聚酸含量的改性环氧树脂涂料。测试了二聚酸改性环氧树脂涂料的力学性能及耐水扩散性。研究结果表明:C36二聚酸改性环氧树脂涂料具有较好的柔韧性、耐冲击性能,以及优良的耐水分子渗透性能。     

Properties and paper sizing application of waterborne polyurethanemicroemulsions: Effects of extender,cross‐linker,and polyol

A series of waterborne polyurethane (WPU) microemulsions were synthesized through self‐emulsification methodology, using toluene‐2,6‐diisocyanate, polytetramethylene glycol (PTMG), poly‐caprolactonediol (PCL), and dimethylol propionic acid (DMPA) as monomers; isophorone diamine (IPDA) as chain extender; and aziridine as cross‐linking agent. The resultant WPU microemulsions were utilized as surface‐sizing agents for cellulose fiber paper. The influences of IPDA content, PTMG/PCL molar ratio, and aziridine content on the physicochemical properties of the resultant emulsions and sized paper have been investigated in detail. The WPU microemulsion displayed better surface sizing properties when it was prepared under the following conditions: the IPDA content of 2.96%, PTMG/PCL molar ratio of 0:4, and aziridine content of 2.0 wt %. The relationships between the WPU structure and properties of WPU films and sized paper were clearly illustrated. The mechanical properties and water resistance of sized paper were not only depended on the interactions, chain entanglements, and cross‐linking density among the WPU chains, but also relied on the interactions among polymers and fibers, as well as the polarity and stiffness of surface sizing agent. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43211.     

合成革用脂肪族聚氨酯树脂的合成

以聚己二酸丁二醇酯二醇(PBA)为软段,异佛尔酮二异氰酸酯(IPDI)、异佛尔酮二胺(IP-DA)和1,4-丁二醇(BDO)为硬段,合成了不合N,N-二甲基甲酰胺(DMF)的弱极性溶剂型脂肪族聚氨酯树脂,考察了软段含量、二次扩链反应温度及nNCO/nOH值对聚氨酯树脂粘度及产品力学等性能的影响.结果表明,软段质量分数在...