三（2-羟丙基）磷酸酯的合成

以磷酸和环氧丙烷为原料直接合成反应型阻燃剂——三(2-羟丙基)磷酸酯。最佳反应条件为:n(H_3PO_4)∶n(环氧丙烷)=1.0∶4.2,反应温度85℃,反应时间为4 h。测试了产品的理化性质。采用红外对其结构进行了表征。热重分析表明,温度600℃时,三(2-羟丙基)磷酸酯的残炭率为16.66%,其稳定性符合材料加工要求,阻燃性能优良。     

三（乙氧基苯基）铋在HTPB推进剂中的应用

通过对端羟基聚丁二烯(HTPB)推进剂的力学性能和燃烧性能测试,探讨了三(乙氧基苯基)铋在不同HTPB推进剂配方中的固化催化作用。结果表明,三(乙氧基苯基)铋对HTPB推进剂体系的催化活性高,能降低固化反应温度,可使推进剂药浆在30～35℃下保温7～9 d完全固化,并使获得的推进剂具有良好的力学性能和燃烧性能。     

阻燃剂三（2，3—二氯丙基）异三聚氰酸酯（TCC）的合成研究

一、前言三(2,3—二氯丙基)异三聚氰酸酯[Tris(2,3—dichloropropyl)isocyanurate,以下简称TCC]全名为1,3,5—三(2,3—二氯丙基)一均三嗪—2,4,6—三酮[1,3,5-Tris-(2,3-dichloropropyl)—s—triazine—2,4,6—trionc],是一种带三嗪环的添加型含氯氮阻燃剂,与高效含溴阻燃剂TBC属同一系列产品。具有优良的阻燃性能、极低的挥发性、良好的相     

硅酸苄基三（氯乙基）酯的合成及表征

以四氯化硅、苯甲醇和环氧乙烷为原料,合成一种硅卤协同阻燃增塑剂硅酸三(氯乙基)苄酯。探讨了反应时间、反应温度以及反应物摩尔比等对产率的影响,筛选出最佳的工艺条件为:n(四氯化硅)∶n(苯甲醇)=1∶1,n(四氯化硅)∶n(环氧乙烷)=1∶3.2,反应温度40℃,反应时间2 h,在该条件下产率为98%。采用FTIR、1HNMR、极限氧指数表征了硅酸三(氯乙基)苄酯的分子结构及性能。     

载Sn（Ⅱ）沸石催化合成偏苯三酸三辛酯

介绍了Sn(Ⅱ)沸石催化剂的制备方法及其在催化合成偏苯三酸三辛酯中的应用，考察了反应温度、时间和催化剂量对反应深度和产品色泽的影响。研究表明，以载Sn(Ⅱ)沸石作为催化剂，通过控制反应条件，可以不经水洗、脱色，得到合格的产品，有效简化了生产工艺。催化剂易于分离，可以重复使用。     

3，5-双（三氟甲基）苯基硅油的合成及性能研究

以3,5-双(三氟甲基)溴苯和甲基三甲氧基硅烷为原料,通过格氏反应和取代反应制备了一种含氟有机硅单体3,5-双(三氟甲基)苯基甲基二甲氧基硅烷;然后将其与二甲基二甲氧基硅烷共水解、平衡聚合制得3,5-双(三氟甲基)苯基硅油.通过FT-IR、1H NMR、19F NMR和元素分析等对含氟有机硅单体和氟硅油进行了表征.含氟硅油的表面张力为20.5 mN/m,大于二甲基硅油(19.0 mN/m).以硅油质量损失10%时的热分解温度来表征材料的热稳定性,二甲基硅油为232.3 ℃,含氟苯基硅油为265.2 ℃,表明含氟苯基硅油的热稳定性比二甲基硅油优越.     

水相合成双-[γ-（三乙氧基硅）丙基]-二硫化物

以γ-氯丙基三乙氧基硅烷(简称γ2)、硫氢化钠、硫为原料,通过加入缓冲剂控制反应体系的pH以抑制γ2的水解,同时运用相转移催化技术,在水相中合成了双-[γ-(三乙氧基硅)丙基]二硫化物(简称Si-75)。主要考察了n(NaHS)∶n(S)、n(γ2)∶n(Na2Sx)、n(Na2CO3)∶n(NaHS)、反应温度、相转移催化剂用量等对合成工艺的影响,最终制得的Si-75外观呈浅黄色,产率为95.4%,w(S)=13.5%。     

动力学拆分制备（R）-3,5-双三氟甲基苯乙醇

通过动力学拆分方法,由3,5-双三氟甲基苯乙酮出发,经过 NaBH4还原,制备得到高纯度消旋化的(R,S)-3,5-双三氟甲基苯乙醇。经过筛选得到2种高效高选择性动力学拆分(R,S)-3,5-双三氟甲基苯乙醇的脂肪酶：Novozym 435和Rhizopus arrhizus。以Rhizopus arrhizus作为实验脂肪酶,考察了影响其动力学拆分的因素,包括溶剂、反应温度和底物浓度,获得最佳的反应条件为：正己烷作为溶剂,40℃下反应,底物浓度为100 mmol/L。在最佳的条件下,以乙酸乙烯酯作为酰基供体进行动力学拆分反应,经过后期的分离纯化,成功制备得到了e.e.值接近100%的(R)-3,5-双三氟甲基苯乙醇。     

偏苯三酸三辛酯（TOTM）增塑剂发展动向

本文介绍性能优异的耐热耐久增塑剂—偏苯三酸三辛酯(TOTM)的生产方法及其同内外市场发展动向。     

聚氨酯涂料讲座（连载三之二）

第三章聚氮醋涂料化学(下) 三、活性氢化合物的反应性聚氨酯涂料用基料,通常都是由二异氰酸酯和活性氢化合物逐步聚合而成的。因此有必要研究活性氢化合物的反应性。一般说来,活性氢化合物的亲核性愈大,愈容易和异     

柠檬酸三丁酯中和水洗实验研究

在柠檬酸三丁酯的产品提纯过程中，粗酯采用先脱正丁醇后中和水洗的方法，易造成乳化，且酸值只能达到0．2mgKOH／g左右。而采用不脱醇就中和水洗的方法，可以避免乳化，并且有效降低产品的酸值至0．05mgKOH／g以下。     

乙酰柠檬酸三丁酯合成工艺的改进

以柠檬酸、正丁醇和乙酸酐为原料,对甲苯磺酸为催化剂,通过酯化、脱醇、乙酰化、脱乙酸和乙酸酐、中和、水洗等步骤制备了乙酰柠檬酸三丁酯。和文献报道的工艺相比,节省了催化剂用量,减少了近一半的废水量。当反应物摩尔比n（柠檬酸）：n（正丁醇）：n（乙酸酐）：n（对甲苯磺酸）=1：4．3：1．10：0．041,酯化反应温度为130-140℃,酯化时间为4h,乙酰化反应温度为50℃,乙酰化反应时间为1h时,产品的产率为97．5％,酯含量为99．21％,酸值为0．14mgKOH／g,色度小于50（Pt—Co）,符合产品质量要求。     

Synthesis of economically viable biodiesel from waste frying oils (WFO)

In present communication, waste frying oil (WFO) has been used as a feedstock for biodiesel synthesis. WFO, procured from a local Indian restaurant possessed an acid value of 0.84 mg KOH/g, which is low enough for single step transesterification reaction. Biodiesel (fatty acid methyl esters) was washed after transesterification reaction and the yield got lowered substantially (from 96% to 86.36%) after water washing owing to loss of esters. 30:100 vol% (methanol to oil), 0.6 wt% NaOCH₃, 60°C temperature and 600 rpm agitation in 1 h reaction time was found to be optimum for transesterification reaction. ¹H NMR spectrum showed a high conversion (95.19%) of fatty acids in WFO to biodiesel in 2 h reaction time. Almost complete conversion (99.68%) was attained in 2 h reaction time. © 2011 Canadian Society for Chemical Engineering     

Production of biodiesel from soapstock using an ion-exchange resin catalyst

The feasibility of biodiesel production from soapstock containing high water content and fatty matters by a solid acid catalyst was investigated. Soapstock was converted to high-acid acid oil (HAAO) by the hydrolysis by KOH and the acidulation by sulfuric acid. The acid value of soapstock-HAAO increased to 199.1 mg KOH/g but a large amount of potassium sulfate was produced. To resolve the formation of potassium sulfate, acid oil was extracted from soapstock and was converted to HAAO by using sodium dodecyl benzene sulfonate (SDBS). The maximum acid value of acid oil-HAAO was 194.2 mg KOH/g when the mass ratio of acid oil, sulfuric acid, and water was 10: 4: 10 at 2% of SDBS. In the esterification of HAAO using Amberylst-15, fatty acid methyl ester (FAME) concentration was 91.7 and 81.3% for soapstock and acid oil, respectively. After the distillation, FAME concentration became 98.1% and 96.7% for soapstock and acid oil. The distillation process decreased the total glycerin and the acid value of FAME produced a little.     

Extraction of yttrium using naphthenic acid with different acid numbers

Naphthenic acid with acid number of 100–200 mg KOH/g could be used to extract yttrium in the system of 20% naphthenic acid + 20% n-butanol + 60% n-hexane. A transparent and uniform phase was formed during saponification but did not influence the extraction process. n-Butanol and n-hexane could shorten phase separation time and lessen emulsification. Excess naphthenic acid and ammonia, and non-naphthenic acid substances contributed to emulsification and difficulty in phase separation, which were especially serious in system of 20% naphthenic acid + 20% 2-octanol + 60% kerosene. Naphthenic acid with acid number <100 mg KOH/g was unsuitable for extraction in either system. Extraction percentages were 99% and 46% when being saponified by 12.7 and 6.3 mol/L ammonia, respectively.     

低黏度氢化蓖麻油聚氧乙烯(40)醚的合成

以氢化蓖麻油和环氧乙烷为原料,三氟化硼乙醚作催化剂,合成了氢化蓖麻油聚氧乙烯(40)醚。产物为极淡黄色,常温下为透明液体,羟值为70~80 mg KOH/g,皂化值为60~70 mg KOH/g,黏度为1 500~2 000 mPa.s。对影响目标产物黏度、色泽、外观、羟值和皂化值的主要因素进行了优化,得到了适宜的反应条件:w(三氟化硼)=0.8%~1.3%,反应温度100~120℃。用500 L反应釜进行扩试生产,得到的产品色泽为极淡黄色,常温下为透明液体,羟值为70.3 mg KOH/g,皂化值为63.2 mg KOH/g,黏度为1 620 mPa.s。     

Purification Process,Physicochemical Properties,and Fatty Acid Composition of Black Soldier Fly (Hermetia illucens Linnaeus) Larvae Oil

This study presented a refining process and reported on fatty acid composition and the physicochemical properties of the oil from black soldier fly larvae (BSFL). Crude larvae oil was purified through four steps consisting of degumming, neutralization, bleaching, and deodorization. Optimum degumming conditions that give the highest phospholipid weight and oil consisted of water concentration of 7% (v/v), followed by addition of H₂SO₄ at a concentration of 0.5% (v/v). Optimum conditions for saponification that maximize saponification value and free fatty acid (FFA) value were 0.4 mg NaOH/100 g oil, 1 hour, and 80 °C of NaOH quantity, reaction time, and temperature, respectively. The oil was then dehydrated using 10 mg Na₂SO₄/g oil. The bleaching process that gives maximum oil yield consisted of activated carbon at concentration of 5% (w/w), followed by centrifugation at a speed of 5000 rpm (radius = 86 mm) for 30 min. The contents of lauric acid, linoleic acid, and linolenic acid in purified oil were 28.8%, 11.1%, and 0.4%, respectively. Physicochemical properties of the refined oil included viscosity of 96 ± 0.14 cP (measured at 20 °C), FFA value of 0.45 ± 0.017%, acid value of 0.9 ± 0.043 mg KOH g⁻¹, saponification value of 215.78 mg KOH g⁻¹, iodine value of 53.7 gI₂/100 g, and peroxide index of 133 mEq kg⁻¹.     

Removal of mineral matter from some Australian coals by Ca(OH)2/HCl leaching

Four Australian coals, Blair Athol, Ebenezer, Newlands and Warkworth coals, were demineralized by Ca(OH)₂ digestion at 300°C, followed by washing with dilute HCl. Ash contents decreased from 8.8–15.4% to 1% for Blair Athol, Newlands and Warkworth coals, and from 14.9% to 2.8% for Ebenezer coal. The CaO/ash ratio is an important factor affecting coal demineralization; the maximum ash removals were achieved at CaO/ash ratios in the range 0.6–1 g/g for all the coals. The major minerals in the original coals were kaolinite and quartz, with some montmorillonite and carbonates. Kaolinite and quartz hydrothermally reacted with Ca(OH)₂ to form calcium-bearing hydrated silicates and aluminosilicates, such as tobermorite and hibschites, that could be dissolved in acid. With increasing CaO/ash ratio in excess of the optimum value, the removal of quartz significantly decreased; there also remains some calcium in treated coal, depending on digestion conditions and coal type. A lower ash removal from Ebenezer is due to a lower quartz removal and more remaining calcium.     

稀土固体超强酸SO4^2—／TiO2／La^3＋催化合成丁酸丁酯

研究了以稀土固体超强酸ＳＯ４＾２－／ＴｉＯ２／Ｌａ＾３＋为催化剂,丁酸和正丁醇为原料合成丁酸丁酯,并考察了影响反应４ 因素。结果表明,醇酸物质的量比为１．８：１,催化剂用量为０．５ｇ（本酸为０．２ｍｏｌ的情况下）,带水剂甲苯为１５ｍＬ,反应时间为２．０ｈ是合成丁酸丁酯的较适宜的反应条件,酯化率达９８．６％。     

Fatty acid composition and physicochemical properties of ostrich fat extracted by supercritical fluid extraction

The objective of this study was to determine the fatty acid composition and physicochemical properties of ostrich fat obtained by supercritical fluid extraction. The fatty acid composition was analysed by GC‐MS and the result revealed that ostrich fat contained 9‐octadecenoic acid (40.7 ± 0.3%), hexadecanoic acid (32.5 ± 0.3%), octadecanoic acid (7.43 ± 0.05%), 9, 12‐octadecadience acid (7.38 ± 0.02%) and 9‐hexadecenoic acid (7.13 ± 0.15%) as the major components. Furthermore, seven physicochemical indexes were assessed according to Chinese Pharmacopeia (2005) and relevant regulations as follows: relative density (0.92 ± 0.02%), melting point (34.7 ± 0.4°C), acid value (0.84 ± 0.02 mg KOH/g), peroxide value (0.10 ± 0.01 g/100 g), saponification value (226 ± 3 mg KOH/g), ester value (225 ± 3 mg KOH/g) and iodine value (74.6 ± 0.8 g I/100 g). It can be inferred from the basic information that ostrich fat is a promising raw material for the pharmaceutical and cosmetics industries. Practical applications : With the increasing attention being paid to ostrich fat, it is necessary to elucidate the fatty acid composition and physicochemical properties of this natural product. This basic information not only reveals the essential characteristics of ostrich fat, but also provides the data support for the quality evaluation and efficacy research.