硼含量对改性酚醛树脂性能的影响

以硼酸作为高羟甲基低游离酚PF(酚醛树脂)的改性剂,制备相应的BPF(硼改性酚醛树脂)及其模塑料。采用红外光谱(FT-IR)法对BPF的结构进行了表征,并对其凝胶化时间、固化工艺条件、热性能和模塑料的性能等进行了探讨。研究结果表明:当w(B)=9%时,BPF及其模塑料的综合性能相对最好,其固化工艺为160℃/20 min,后处理工艺为"140℃/1 h→160℃/1 h→180℃/2 h";与纯PF模塑料相比,BPF模塑料的马丁耐热温度(196℃)提高了42℃、弯曲强度(111.8 MPa)提高了21.9 MPa且冲击强度(18.50 kJ/m2)也有所提高。     

硼-腰果酚改性酚醛树脂的制备及固化动力学

针对酚醛树脂(PF)耐热性和韧性不足的缺点,采用硼、腰果酚对酚醛树脂进行改性,考察了硼酸用量和腰果酚用量等对改性酚醛树脂性能的影响。红外(FT-IR)分析结果表明,硼酸与酚醛树脂中的酚羟基发生了反应,生成了新的交联键。通过热重(TG)分析,结果表明经硼改性的酚醛树脂耐热性能明显提高。通过非等温差示扫描量热法(DSC)分析了改性酚醛树脂在不同升温速率下的固化行为,采用Ozawa法和Crane方程建立了改性酚醛树脂的固化动力学模型,确定了其固化工艺参数。     

硼改性酚醛树脂的合成与性能

利用半成品酚醛树脂粉与硼酸直接混合,然后固化得到硼含量不同的硼酚醛树脂,并用傅里叶红外光谱、热重分析和冲击试验等方法对其性能进行了分析。红外分析结果表明,硼酸与酚醛树脂中的酚羟基、苄羟基发生了反应,生成了新的交联键。热分析结果发现,在酚醛树脂中加入硼酸能提高树脂的耐热性,当硼酸加入量为10%时达到最高值。硼酚醛树脂的冲击强度先随硼酸加入量的增大而增加,在5%时达到最大值,然后下降。     

新型催化合成法制备硼改性酚醛树脂的研究

以硼酸钾为催化剂一步法合成硼酚醛树脂,硼酸钾既是催化剂也是酚醛树脂的改性剂。用IR和TGA对生成物进行了表征。探讨了酚醛摩尔比、不同催化剂加入量和反应时间对产物各项性能的影响。最佳酚醛摩尔比为1.75,硼酸钾摩尔比为0.2,最佳反应时间为13小时。     

原位生成SiO_2改性硼硅酚醛树脂的合成与性能研究

在合成酚醛树脂的过程中引入有机硅预聚物和硼酸,制得硼硅酚醛树脂,并在此基础上加入正硅酸乙酯,原位水解生成SiO 2,进一步改性了硼硅酚醛树脂。分别考查了有机硅预聚物、硼酸和正硅酸乙酯加入量对改性酚醛树脂粘接强度的影响。通过IR考查了改性树脂的结构,硼氧键和硅氧键成功地引入到酚醛树脂中。还通过DSC和不同条件下粘接强度的测试考查了改性树脂的固化性能,确定了其固化工艺。空气气氛中的热重分析则表明改性酚醛树脂初始分解温度为475℃,1 000℃残炭率为21%,耐热性明显优于普通酚醛树脂。     

烯丙基醚化程度对BMI改性PF模塑料性能的影响

先将线性酚醛树脂(PF)烯丙基醚化,再用双马来酰亚胺(BMI)改性烯丙基醚化的线性PF(AEN),得到AEN/BMI共聚物(BAN),通过傅立叶变换红外光谱、凝胶化时间和差示扫描量热分析分别分析了BAN的结构和固化工艺,测试了不同烯丙基醚化程度的BAN模塑料的耐热性、电性能和力学性能。结果表明,当固化剂为六次甲基四胺时,模压温度为160℃、后处理工艺为140℃/1 h+150℃/1 h+160℃/2 h、烯丙基醚化程度为36.5%时,BAN模塑料的综合性能最佳。     

本期特约专栏主持人——张斌教授：原位生成SiO2改性硼硅酚醛树脂的合成与性能研究

在合成酚醛树脂的过程中引入有机硅预聚物和硼酸,制得硼硅酚醛树脂,并在此基础上加入正硅酸乙酯,原位水解生成SiO2,进一步改性了硼硅酚醛树脂。分别考查了有机硅预聚物、硼酸和正硅酸乙酯加入量对改性酚醛树脂粘接强度的影响。通过IR考查了改性树脂的结构,硼氧键和硅氧键成功地引入到酚醛树脂中。还通过DSC和不同条件下粘接强度的测试考查了改性树脂的固化性能,确定了其固化工艺。空气气氛中的热重分析则表明改性酚醛树脂初始分解温度为475℃,1000℃残炭率为21％,耐热性明显优于普通酚醛树脂。     

含硼硅酚醛树脂的制备及耐热性研究

酚醛树脂由于成型工艺简单、成本低和具有优异耐烧蚀性能而被广范应用于航空航天和武器装备等领域。为了进一步提高酚醛树脂的耐热性，分别采用两种方法制备含硼硅酚醛树脂，研究发现，分两步将硼元素和硅元素分别以B—O—C结构和Si—O—B耐高温结构引入酚醛树脂中，制备的含硼硅酚醛树脂耐热性和力学性能均得到改善。通过研究发现，相比于未改性酚醛树脂，含硼硅酚醛的耐热性、层间剪切强度和弯曲强度均提高，当使用甲基三乙氧基硅烷制备含硼硅酚醛树脂时，其固化物在T_5%、T_10%、T_max和R_800℃分别为416.13℃、543.62℃、567.11℃和75.99%，分别提高了95.7℃、104.5℃、29.3℃和17.94%。制备的玻璃纤维增强含硼硅酚醛树脂复合材料的层间剪切强度从16.8 MPa增加至28.6 MPa，弯曲强度从132.5 MPa提高至261.9 MPa。     

硼改性酚醛泡沫的耐高温性能

本文以添加硼酸的方法,通过控制体系的pH值,合成可发泡的硼改性酚醛树脂,并制备出硼改性酚醛泡沫。测试表明,该材料具有良好的耐高温性能,其热分解温度为450℃,800℃热失重为60%,最高使用温度为200℃。同时探讨体系pH值对硼改性酚醛树脂可发性和稳定性的影响,分析硼改性提高酚醛泡沫耐高温性能的原因。     

酚醛型氰酸酯的性能

表征了采用"改进的卤化氰-酚法"合成得到的酚醛型氰酸酯未固化树脂的粘度、反应性和凝胶特性,固化树脂及其复合材料的力学性能、耐热性、耐烧蚀性能等。结果表明,固化气氛对酚醛型氰酸酯的反应活性有着显著的影响,在空气气氛中的凝胶时间远小于惰性气氛的凝胶时间。固化树脂及其复合材料具有优异的耐热性和烧蚀残留率,力学性能优于酚醛树脂。     

青霉素菌丝中蛋白质酶法水解工艺

采用碱热法溶解青霉素菌丝,研究酶法催化水解菌丝溶解液中蛋白质转化为氨基酸的过程.考察酶种类、溶解液pH值、酶与蛋白质质量比、反应温度和时间等因素对蛋白质水解度的影响,建立最佳水解工艺.结果 表明,酶种类、酶与蛋白质之比、pH、温度和时间均对蛋白质水解过程产生影响.以单酶为催化剂,碱性蛋白酶催化水解效果最好,蛋白质水解度...     

Synthesis of MAG of CLA with Penicillium camembertii lipase

CLA has various physiological activities, and a FFA mixture containing almost equal amounts of cis-9,trans-11 and trans-10,cis-12 CLA (named FFA-CLA) has been commercialized. We attempted to produce MAG of CLA by a two-step successive reaction. The first step was esterification of FFA-CLA with glycerol. A mixture of FFA-CLA/glycerol (1∶5, mol/mol), 2 wt% water, and 200 units/g of Penicillium camembertii mono-and diacylglycerol lipase was agitated at 30°C to form a homogeneous emulsion. The esterification degree reached 84% after 10 h. To further increase the degree, the reaction was continued with dehydration at 5 mm Hg. The esterification degree reached 95% after 24 h (34 h in total), and the reaction mixture contained 50 wt% MAG and 44 wt% DAG. The second step was glycerolysis of the resulting DAG. The reaction mixture in the first-step esterification was transferred from the reactor to a beaker and was solidified by vigorous agitation on ice. When the solidified mixture was allowed to stand at 5°C for 15 d, glycerolysis of DAG proceeded successfully, and MAG content in the reaction mixture increased to 88.6 wt%. Hydrolysis of the acylglycerols was not observed during the second reaction. FA composition in the synthesized MAG was completely the same as that in the original FFA-CLA, showing that Penicillium lipase does not have selectivity toward FA in the FFA-CLA preparation.     

3-溴苯酞合成工艺的研究

对3～溴苯酞的几种合成方法进行了比较。研究了以邻甲基苯甲酸为原料舍成3-溴苯酞的工艺,较好的工艺条件是邻甲基苯甲酸和溴素的摩尔比为1：2,反应温度140℃,滴加溴素,7．6h完成溴化过程,采用二氯乙烷作重结晶溶剂,产品总收率78．64％,含量98．71％。尾气冷凝器二台并联设置,解决尾气管道堵塞的问题。尾气吸收采用二级降膜吸收加一级碱液吸收的设置,回收的溴化氢含量≥35％。采用自制干燥剂保存产品。     

阻燃剂季戊四醇双磷酸酯二磷酰氯缩三聚氰胺的合成及表征

以季戊四醇、氧氯化磷、三聚氰胺为原料,两步合成了阻燃剂季戊四醇双磷酸酯二磷酰氯缩三聚氰胺,通过红外光谱及元素分析对其结构进行了鉴定。最佳合成工艺条件为:第一步,n[C(CH2OH)4]∶n(POCl3)=1∶2.2,反应7 h,反应温度80℃,收率为88%;第二步,n(中间体)∶n(C3N6H6)=1∶2,反应0.5 h,反应温度80℃,收率98%。     

Study of the acid pretreatment and biodiesel production from olive pomace oil

The objective of this work was to study the two‐step acid base homogenous catalyzed transesterification of olive pomace oil, with the ultimate purpose of producing biodiesel under mild reaction conditions by optimizing the process. Optimization of the experimental procedure was conducted by a factorial design of 2³ under the acidic pretreatment step and during the basic transesterification. The optimal production of methyl esters (97.8%) was achieved for the experimental conditions H₂SO₄ = 20 wt%/CH₃OH = 35:1/T = 40^°C and KOH = 0.6+ fatty acid value /CH₃OH = 9:1/ T = 60^°C, in the acidic and basic stage of the process, respectively. Finally, to properly assess the quality of the biofuel produced, it was tested for all the European Standard properties.     

甲基丙烯酸十六酯-乙酸乙烯酯低温流动性能改进剂的研制

以甲基丙烯酸、十六醇、乙酸乙烯酯为原料,用先酯化后聚合法设计并合成了甲基丙烯酸十六酯-乙酸乙烯酯共聚物,用作柴油低温流动性能改进剂。得到了制备该聚合物的最优反应条件,酯化:n甲基丙烯酸∶n十六醇=1∶1、w对甲苯磺酸=1.8%(以酸醇总质量计,下同),w二甲苯=105%、酯化时间90 min;聚合:w乙酸乙烯酯=30%,w过氧化苯甲酰=1.8%,反应时间4 h,反应温度80℃。改进剂加剂量9 490μg/g时,可使自制0#柴油冷滤点下降11℃。     

超细h-BN粉在无水乙醇介质中复合分散工艺研究

针对超细h-BN粉体易团聚、与有机基体界面相容性较差的缺点,研究了其在无水乙醇介质中的分散工艺.首先在测定其pH-Zeta电位的基础上,选取阴离子型(SA、OA、SDBS)、非离子型(PVP、KH570、司班85)和高分子型(PEG4000)分散剂进行超声分散研究.然后从以上几种分散剂中选取三种分散剂进行复合分散.实验发现:在最佳配比下,复合分散体系较单分散剂分散效果明显提升,PEG4000与SA的复合分散比最佳单分散剂的效果提升了18%;KH570与SA的复合分散体系比最佳单分散剂的效果提升了11%;推荐h-BN粉在无水乙醇中的分散工艺为:pH值为9时,在560 W的功率下用SA(4wt%)与PEG4000(1wt%)或者SA(1wt%)与KH570(4wt%)复合超声90 min.     

BPR含量对BPR/SF/PF复合材料摩擦磨损性能和力学性能的影响

将硼酚醛树脂(BPR)与普通酚醛树脂(PF)熔融共混,再加入经过碱处理的剑麻纤维(SF),通过模压成型工艺制备BPR/SF/PF复合材料。利用定速式摩擦试验机和电子万能试验机研究了BPR含量对复合材料摩擦磨损性能及力学性能的影响,采用扫描电镜观察了复合材料磨损表面的形貌。结果表明:在BPR/PF=50/100时,与普通PF/SF复合材料相比,BPR/SF/PF复合材料在300℃下的磨损率降低了42%,冲击强度提高了14%,弯曲强度和弯曲模量分别提高了25%和36%;复合材料磨损面形貌显示,加入BPR后,复合材料由疲劳磨损转变为磨粒磨损。     

A lightweight CNWs-SiO2/3Al2O3·2SiO2 porous ceramic with excellent microwave absorption and thermal insulation properties

To obtain excellent microwave absorption and thermal insulation properties, carbon nanowires reinforced SiO₂/3Al₂O₃·2SiO₂ composite ceramics (CNWs-SiO₂/3Al₂O₃·2SiO₂) were fabricated by catalytic chemical vapor deposition (CCVD) using C₂H₄ as the carbon source. The content of CNWs in SiO₂/3Al₂O₃·2SiO₂ porous ceramics can be adjusted by controlling the concentration of the catalyst precursor and the CCVD time. A higher concentration of catalyst precursor and longer CCVD time are beneficial for the growth of CNWs and for improving the electromagnetic wave (EMW) absorption properties of CNWs-SiO₂/3Al₂O₃·2SiO₂. However, CNWs are harmful to impendence matching due to the strong reflection and weak absorption when the content exceeds the threshold (30 wt%) in SiO₂/3Al₂O₃·2SiO₂ porous ceramics. CNWs are also harmful to the thermal insulation properties due to their high thermal conductivity. The results show that CNWs-SiO₂/3Al₂O₃·2SiO₂ can attain good EMW absorption and thermal insulation properties if the content of CNWs is 30 wt% when the concentration of the catalyst precursor is 3 wt% and the CCVD time is 15 min. The effective absorption bandwidth (EAB) can cover from 8.2 to 12.4 GHz (the whole X-band), and the minimum reflection coefficient (RC_min) is -31 dB at 9.1 GHz. The temperature gradient is 218 °C, which can satisfy the design requirement. Thus, the dielectric and thermal insulation properties are designable for CNWs reinforced SiO₂/3Al₂O₃·2SiO₂ porous ceramics to obtain excellent EMW absorption and thermal insulation properties.     

Rapid one-pot synthesis of SiO2@SiO2/Carbon@Carbon core-shell composites with efficient microwave absorption in a short time

A carbon-silica nanomaterial for electromagnetic wave (EW) absorption was synthesized using a modified one-pot method. The unique hydrolysis-polymerization process forms a SiO₂@SiO₂/Carbon@Carbon core-shell structure. The growth process of the material was studied by transmission electron microscope (TEM) and thermogravimetric analysis (TGA). Nanoparticles were successfully synthesized with a core-shell structure after 6 h of reaction, and the composite material showed excellent EW absorption performance with a thickness of 3.8 mm. The minimum reflection loss (RL_min) was ?56.3 dB, and the broadest effective absorption bandwidth (EAB) (RL ≤ 10 dB, 90% absorption) covered 5.15 GHz (12.48–17.63 GHz) with 1.8 mm of thickness. There is no significant difference in the EW absorption performance with increasing reaction time. Thus, this study provides a method for synthesizing EW-absorbing materials with shorter reaction time, simpler process, and excellent absorption properties, possibly a candidate for further application.