GC-MS测定乌参中多环芳烃残留

建立了气相色谱-质谱法（GC-MS）同时测定乌参中20种多环芳烃残留的方法。样品经蒸馏水混合和二氯甲烷萃取,浓缩,硅胶层析柱净化,外标法定量。20种多环芳烃得到较好的分离,回收率为92.0%~103.0%,相对标准偏差（RSD）为1.86%~4.62%,检出限10μg/kg。实验结果表明,该方法简单、快速、重现性好,能满足乌参中多环芳烃残留的测定要求。     

国内外抽出油的综合利用研究进展

抽出油是润滑油溶剂精制工艺过程中生产的副产物,其中含有大量的芳烃,但常作为燃料油的调合组分,经济效益较低。为充分利用该重质芳烃油资源,生产高附加值产品,实现炼油厂经济效益最大化,本文介绍了国内外溶剂抽出油在环保型橡胶填充油、沥青改性、油墨溶剂油、导热油、绝缘油、缩合多环芳烃树脂等方面的研究与应用。最后并对抽出油的综合利用生产环保型产品提出了展望。     

TCDTO-1重整混合芳烃脱烯烃精制剂的工业应用

国内外大多数装置采用活性白土脱除重整生成油中的烯烃,但活性白土寿命短、需频繁更换,不利于安全生产和环保。考察了TCDTO-1重整混合芳烃脱烯烃精制剂在某石化炼油部重整装置上的工业应用,结果表明,采用布袋装填法,装填密度为0.532 t·m^-3,在反应温度（135～190） ℃、反应压力（0.9～1.0） MPa、空速（0.85～0.95） h^-1、原料溴指数（900～1 600） mgBr·（100g）^-1的工况下,TCDTO-1精制剂性能优越,在不改变原生产工艺、且前端白土塔未进行更换的前提下,溴指数长期稳定在15 mgBr·（100g）^-1以下。使用256天后按计划卸出再生,单程寿命超过白土的13倍,给企业带来可观的经济效益和社会效益。     

Lurgi MTP工艺循环烃组分分布研究

采用气相色谱仪对德国Lurgi MTP工艺的C4循环烃进行分析,并从MTP催化剂运行周期方向考察了循环烃的组分变化规律。分析结果表明,C4循环烃主要组分是烷烃,约占其总物质的量的57%,其余组分为烯烃和少量的甲醇、二甲醚;其中,各组分含量大小为:异丁烷异丁烯正丁烷1-丁烯反-2-丁烯。     

降解含硫杂环芳烃中度嗜盐菌的筛选及降解特性研究

从胜利油田石油污染土壤中筛选分离出6株对二苯并噻吩具有降解能力的中度嗜盐菌,其中SL-4菌株的降解效果最好,在底物浓度为50 mg·L-1、培养基盐度为5％条件下对二苯并噻吩的降解率达到37.2％.通过单因素实验考察了底物初始浓度、pH值、温度、氮磷比对SL-4菌株降解效果的影响.正交实验结果表明：氮磷比是影响SL-4菌株降解效果的主要因素,其次是pH值和温度;SL-4菌株的最佳培养条件为：pH值7.5、温度25℃、氮磷比6∶1.     

对羟基偶氮苯甲酸的合成及光致变色性能研究

研究对羟基偶氮苯甲酸(PHABA)的合成方法及其光响应性能。在低温盐酸条件下,完成对氨基苯甲酸与亚硝酸钠的重氮化反应,再与苯酚pH=9条件下完成偶合反应,产品收率82.6%。氯仿溶剂中,PHABA特征吸收波长为357 nm和240 nm,紫外光照射实验显示,PHABA具备动力学一级反应特征的顺反异构光致变色特性,速率常数为7.46×10-4 min-1。     

Comparing the corrosivity of acidic species in petroleum fractions by raman spectroscopy,energy-dispersive spectrum and scanning electron microscopy

The main object of this work was to compare the corrosion powers of acidic species: naphthenic acid, fatty acid and aromatic acid which were found in petroleum fraction. They were blended into base oils to formulate three simulate oils (E, F and G) with the same TAN values of 2.3 mg KOH/g. AISI 316 steel surfaces immersed in oils were measured by Raman spectroscopy, energydispersive spectrum and scanning electron microscopy after 24, 48, 72 h to evaluate their corrosion. From the Raman images, the corrosion products were confirmed. Besides goethite (α-Fe(OOH)) in corrosion product E at 48 hours; magnetite (Fe₃O₄) in F at 24 hours; and hematite (α-Fe₂O₃ and α-Fe₂O₃) in G at 72hours, there were disordered carbons on steel E and ferric benzoate film on steel G. The contents of elements from EDS have markedly different characteristics, indicating that dominant corrosion products on steel samples resulted from three acidic species are different. The morphology in SEM also corroborated above data that corrosion products have difference. Combining the data of three measurements, the rank of corrosion power based on the formations of ferric oxides was determined: fatty acid > naphthenic acid > aromatic acid.     

高黏度聚α-烯烃合成油加氢技术研究

采用中国石油石油化工研究院开发的Pt-Pd/Al_2O_3加氢精制催化剂对聚α-烯烃PAO40粗产品进行了加氢精制。结果表明:在反应温度240~280℃、反应压力4.0~8.0 MPa、体积空速0.1~0.4h-1、氢油体积比300∶1的工艺条件下,PAO40加氢产品的芳烃含量达到国外同类优秀产品水平;PAO40加氢产品经光照30天后不变色,具有较好的光安定性。     

Palladium‐Catalyzed Carbonylative Synthesis of 2,3‐Disubstituted Chromones

An unexpected palladium‐catalyzed carbonylative synthesis of 2,3‐disubstituted chromones has been developed. Starting from 2‐bromofluorobenzenes and ketones, the corresponding chromones were produced in good yields. By control experiments, this transformation was found to proceed through a sequential carbonylation/Claisen–Hasse rearrangement/intramolecular nucleophilic aromatic substitution approach (S_NAr). More specifically, the reaction sequence started with a palladium‐catalyzed carbonylation of the ketone with o‐bromofluorobenzene to give the vinyl benzoates, which subsequently transformed into 1,3‐diketones via a Claisen–Hasse rearrangement. The final products were produced after an intramolecular S_NAr reaction of the in situ formed 1,3‐diketone.

     

Visible Light‐Initiated C(sp3)?Br/C(sp3)?H Functionalization of α‐Carbonyl Alkyl Bromides through Hydride Radical Shift

A new visible light‐initiated 1,5‐hydride radical shift strategy has been developed to enable the one‐step functionalization of both a C(sp³) Br bond and a C(sp³) H bond adjacent to the same carbon atom. This visible light photoredox catalysis offers a mild and straightforward access to diverse five‐membered carbocyclic ring‐fused polycyclic hydrocarbons with high turnover numbers (TONs; up to 4.93×10³) and broad substrate scope.