脱水磷酰氯法合成磷酸二异辛酯

研究了脱水磷酰氯法合成磷酸二异辛酯的新方法。先以五氧化二磷和二氯亚砜反应制备了脱水磷酰氯,脱水磷酰氯再与异辛醇反应制得目标产物磷酸二异辛酯。考察了磷酰氯与异辛醇物质的量比、异辛醇的滴加温度、反应时间、反应温度和真空度等关键因素对反应的影响。实验结果表明,n(脱水磷酰氯)∶n(异辛醇)=1.0∶2.1、15℃下滴加异辛醇、60℃下反应3 h、真空度为0.08 MPa的条件下,磷酸二异辛酯的收率达96.2%,含量达97.9%。利用FT-IR和NMR对产物磷酸二异辛酯进行表征。     

固体超强酸催化合成氯乙酸异辛酯

以自制固体超强酸为催化剂,以氯乙酸和异辛醇为原料合成氯乙酸异辛酯。考察了催化剂用量、反应物料物质的量的比、带水剂用量及反应时间对酯化反应的影响。实验结果表明,TiO2-SO4^2-类固体超强酸具有良好的催化性能,反应最佳条件为：氯乙酸用量为0．15mol时,n（异辛醇）：n（氯乙酸）=1,1：1．0,催化剂质量分数为反应物的质量的1．2％,带水刺为10mL,反应时间为2．5h。在此条件下,氯乙酸异辛酯的收率达98％,且催化剂重复使用5次。氯乙酸异辛酯的收率无明显下降。     

硬脂酸异辛酯的合成

叙述了采用硬脂酸与异辛醇进行酯化反应,合成硬脂酸异辛酯的方法。中试产品经测试及有关工厂使用,可取代进口产品。     

利用纳米氧化物辅助制备十六烷值改进剂的方法

本文报道了利用纳米氧化铜辅助制备十六烷值改进剂的方法:以硝酸和异辛醇为原料,硫酸为催化剂,纳米氧化铜为辅助稳定剂,在最佳实验条件下,合成了柴油十六烷值改进剂—硝酸异辛酯。结果表明,硫酸与硝酸的质量比为1.0:1,硝酸与异辛醇的质量比为1.8:1,酯化温度25℃,酯化反应时间60min,纳米氧化铜的加入量为异辛醇使用量的0.3%。在此条件下,反应比较平稳、安全。产品经红外光谱和气相色谱分析,合成产物与目标产物结构完全一致,得到硝酸异辛酯的产率为98.5%和纯度为99.8%。该方法克服了十六烷值改进剂合成工艺的安全系数低、反应过程不稳定以及副产物难除去等缺陷,有助于进一步提升了产品的性能和指标。     

新型磷类结焦抑制剂中间体的合成研究

乙烯裂解生产过程中存在的一个突出的问题是结焦,磷酸二异辛酯的吗啉盐是一种新型的结焦抑制剂。实验就是以磷酸和异辛醇为原料,通过改变催化剂的种类、酸醇比、催化剂用量、反应时间等合成磷酸二异辛酯。实验得到合成磷酸二异辛酯的最佳条件为以钨磷酸为催化剂,催化剂用量为原料质量的2.0%,异辛醇与磷酸摩尔比为2.3,反应时间为4 h。此时磷酸二异辛酯收率可达72.8%。     

微通道反应器连续法合成硝酸异辛酯

以硝硫混酸作为硝化剂,与异辛醇在微通道反应器中经硝化反应得到硝酸异辛酯。考察了反应温度、混酸配比、硝酸浓度、停留时间、反应物配比对产品收率的影响,优化出微通道反应器中合成硝酸异辛酯的适宜工艺条件,硝酸异辛酯的收率97.8%,纯度达99.5%。微通道反应器连续法合成硝酸异辛酯具有操作简单、反应时间短、收率高、安全可靠等优点,具有工业化应用前景。     

二丁基氧化锡催化酯交换合成硬脂酸异辛酯的研究

以硬脂酸甲酯和异辛醇为原料,二丁基氧化锡(n-Bu2SnO)为催化剂,通过酯交换法合成了硬脂酸异辛酯。考察了反应温度、催化剂用量,反应时间及物料配比等因素对酯交换反应的影响,并考察了催化剂重复使用情况。常压下,反应温度为140℃,n-Bu2SnO与硬脂酸甲酯的摩尔比0.011 4∶1,硬脂酸甲酯与异辛醇摩尔比1∶1.5,反应2 h条件下,硬脂酸异辛酯收率达到89.0%。n-Bu2SnO循环使用5次后,催化活性基本不变。对反应前后n-Bu2SnO的IR和XRD结构表征表明它具有很好的稳定性。     

催化合成氯乙酸异辛酯的研究

以氯乙酸和异辛醇为原料，用催化剂NS催化合成氯乙酸异辛酯，探讨了酯化反应的条件。当n(异辛醇)／n(氯乙酸)为1．1：1、催化剂用量占反应物料质量的2．5％时，反应2h，氯乙醇异辛酯的收率达到94．7％。     

钛酸四丁酯催化合成氰乙酸异辛酯的研究

以氰乙酸乙酯和异辛醇为原料,采用钛酸四丁酯为催化剂,用酯交换法合成氰乙酸异辛酯。考察了原料配比、反应温度、催化剂用量等对反应产率的影响。指出了合成氰乙酸异辛酯的优化条件：n(氰乙酸乙酯)／n(异辛醇)为1：1．10,催化剂用量为5．0g,反应温度为150℃,在此条件下氰乙酸异辛酯反应产率为94．38％(以氰乙酸乙酯计)。     

废聚酯制备对苯二甲酸二异辛酯工艺条件的研究

对苯二甲酸二异辛酯(DOTP)是一种环保、安全无毒的增塑剂。本实验采用聚酯废料与过量异辛醇采取醇解酯交换法制备对苯二甲酸二异辛酯(DOTP)的方法,利用在不同反应条件下产品的产率,综合产品的pH值、粘度、颜色,确定最佳的反应条件。当反应条件:聚酯废料与异辛醇物质的量比1∶4,催化剂采用原料量的0.4%的醋酸锌与钛酸四丁酯1∶1混合催化剂,反应温度为200～210℃,反应时间为7h时,对苯二甲酸二异辛酯(DOTP)收率最高为86%。     

磷酸二异辛酯的合成研究

乙烯裂解生产过程中存在的一个突出的问题是结焦,磷酸二异辛酯的吗啉盐是一种新型的结焦抑制剂.本实验就是以磷酸和异辛醇为原料,通过改变催化剂的种类、酸醇比、催化剂用量、反应时间等条件来合成磷酸二异辛酯.钨磷酸含量为5.0％时催化剂活性最好;产品收率随催化剂用量的增大而提高,当催化剂用量超过2.0％时,产品收率基本不变;增大...     

用异辛醇合成磷酸酯

以磷酸和异辛醇为原料,在自制活性三氧化二铝催化剂条件下经酯化、水洗、干燥、减压蒸馏,最终获得产品磷酸三异辛酯.通过改变原料的醇酸摩尔比、催化剂对收率的影响进行研究.结果表明:随着原料的醇酸摩尔比的增大,产物收率逐渐增大,到3.3时趋于稳定;使用Al2O3作催化剂Na2SO4为助催化剂比单独使用Al2O3作催化剂,所得产物收率较高.     

Effect of oxygen donor alcohol on nonaqueous precipitation synthesis of alumina powders

Monodispersed alumina powders were prepared via nonaqueous precipitation process using aluminum powders as aluminum source, acetic acid as precipitant. Effect of oxygen donor and solvent alcohol such as methanol, ethanol, isopropanol on the preparation of ultrafine alumina powders and the precursor reaction mechanism have been investigated by XRD, FT-IR, TEM, FE-SEM and performance tests of sintered bodies. The intermolecular condensation of methanol with the catalysis of Lewis acid aluminum methoxide leads to hydrolysis of aluminum methoxide, forming amorphous precipitates, dehydration polycondensation of aluminum hydroxide and resulting in serious agglomeration of precipitates and alumina powders, the worst morphology and properties of sintered body. The pulling electron effect and steric hindrance of isopropyl group make the structure of aluminum isopropoxide overwhelmingly stable and relatively arduous to be replaced by precipitant acetic acid, which results in underdeveloped crystallinity and agglomeration of both precipitates and alumina powders, poor morphology and properties of sintered body. The optimized oxygen donor and solvent alcohol is ethanol. Monodispersed, high crystallinity C₄H₇AlO₇ precipitates and alumina powders can be obtained when ethanol is used as oxygen donor and solvent, and the highest relative density, mechanical properties and the most homogeneous microstructure was obtained. The density, flexural strength, volume resistivity, breakdown voltage and thermal expansion coefficient are 99.1% of TD, 128.0?±?2.2?MPa, 9.8?×?10¹⁶ Ω?cm, 45.2?kV/mm and 7.6?×?10^?6 °C^?1, respectively. Precursor reaction mechanism is deduced that aluminum powders react with oxygen donor alcohol to form aluminum alkoxide with the catalyst iodine, and then react with acetic acid to form crystal C₄H₇AlO₇ precipitates. Nonaqueous precipitation method is expected to become a promising candidate for mass production of alumina powders.     

Synthesis and Characterization of Amorphous Nano‐Alumina Powders with High Surface Area for Biodiesel Production

Nano‐alumina powders containing yttrium oxide were synthesized via the sol‐gel method using aluminum chloride hexahydrate as catalyst precursor. Fourier transform infrared analysis showed the presence of Al‐O and Al‐O‐Al bands in the powder structure and X‐ray diffraction spectra proved that the alumina was in the amorphous phase. The amorphous nano‐alumina powders were shown to be mesoporous with a high surface area, and both spherical and slit‐shaped particles were found in the calcined powder. A high percentage of conversion of oil to biodiesel was obtained in the transesterification reaction and the synthesized nano‐alumina powders could be easily regenerated for further use. The amorphous nano‐alumina powder can thus be recommended for use as active catalyst in the transesterification reaction for biodiesel production on the industrial scale.     

一水硫酸氢钠催化合成混合二元酸二辛酯

在一水硫酸氢钠催化剂作用下,以异辛醇及生产环己酮的副产混合二元酸为原料,考察了混合二元酸二辛酯合成的工艺条件。结果表明,最佳酯化反应条件为混合二元酸粗品14.6 g,异辛醇40 mL,以15 mL二甲苯作带水剂,催化剂一水硫酸氢钠0.30 g,110～156℃回流反应1.5 h。在该优化条件下,混合二元酸的酯化率达99.64%。催化剂经重结晶后可重复使用。     

Synthesis of aluminum isopropoxide from aluminum dross

Synthetic reaction of aluminum isopropoxide, which is used as a starting material for catalytic-grade alumina, has been studied in the presence of a small amount of HgI₂, HgCl₂, I₂ or FeCl₃ from aluminum dross. It was synthesized by solid-liquid reaction between the aluminum metal and isopropyl alcohol, using vacuum distillation process. The purity of the synthesized aluminum isopropoxide was obtained over 97.6% experimentally, which had been analyzed quantitatively by complexometric method. The initial amount of sodium, which directly affects the catalytic activation in the alumina catalyst, was in the range of 0.926 to 1.563 wt% in the aluminum dross. Finally, it was decreased to 0.007 wt% in the aluminum isopropoxide product. Yield was changed according to the amount of aluminium existing in the aluminum dross. Aluminum could mostly be recovered regardless of the amount of aluminium existing in the aluminum dross.     

PREPARATION OF ULTRAFINE Al 2 O 3 USING PLASMA JET AND ITS APPLICATION FOR SYNTHESIS OF DIMETHYL CARBONATE

A direct preparation of Al 2 O 3 from aluminum and oxygen under plasma jet conditions has been performed in this work. The XRD characterization of such plasma-prepared alumina shows that a production of δ-Al 2 O 3 has been achieved. The size of the alumina particles ranged from several tens to 200 nm, based on SEM analysis. The effectiveness of plasma-prepared alumina as a catalyst support has been demonstrated by the catalytic synthesis of dimethyl carbonate over Pd/Al 2 O 3 .     

Preparation of Mesoporous Ni–alumina Catalyst by One-step Sol–gel Method: Control of Textural Properties and Catalytic Application to the Hydrodechlorination of o-dichlorobenzene

Mesoporous Ni–alumina catalysts (Ni–alumina-pre and Ni–alumina-post) were synthesized by one-step sol–gel method using micelle complex comprising lauric acid and nickel ion as a template with metal source and using aluminum sec-butoxide as an aluminum source. The Ni–alumina catalysts showed relatively high surface areas (303 m²/g for Ni–alumina-pre and 331 m²/g for Ni–alumina-post) and narrow pore size distributions centered at ca. 4 nm. Highly dispersed Ni particles were observed in the Ni–alumina catalysts (ca. 5.2 nm for Ni–alumina-pre and ca. 6.8 nm for Ni–alumina-post) after reduction at 550 °C, while a catalyst prepared without a template (NiAl-comp) exhibited inferior porosity with large metal particles (ca. 12.3 nm). Mesoporous Ni–alumina catalysts with different porosity were obtained by employing different hydrolysis step of aluminum source. When aluminum source was hydrolyzed under the presence of micelle complex, a supported Ni catalyst with highly developed framework mesoporosity was obtained (Ni–alumina-post). On the other hand, when aluminum source was pre-hydrolyzed followed by mixing with micelle solution, the resulting catalyst (Ni–alumina-pre) retained high portion of textural porosity. It was revealed that the hydrolysis method employed in this research affected not only textural properties but also metal-support interaction in the Ni–alumina catalysts. It was also found that the Ni–alumina-pre catalyst exhibited weaker interaction between nickel and alumina than the Ni–alumina-post, leading to higher degree of reduction in the Ni–alumina-pre catalyst. In the hydrodechlorination of o-dichlorobenzene, the Ni–alumina catalysts exhibited better catalytic performance than the NiAl-comp catalyst, which was attributed to higher metal dispersion in the Ni–alumina catalysts. In particular, the Ni–alumina-pre catalyst showing 1.5 times higher degree of reduction and larger amounts of o-dichlorobenzene adsorption exhibited better catalytic performance than the Ni–alumina-post catalyst.     

乙烯聚合铝改性铬系催化剂研究进展

综述国内外乙烯聚合铝改性铬系催化剂的研究现状、制备方法、性能以及对乙烯聚合性能的影响。铝改性铬系催化剂主要体现为采用氧化铝和磷酸铝作为载体,或使用烷基铝作为改性剂。改性后铬系催化剂的聚合活性和氢调敏感性明显提高,由其生成聚合物的相对分子质量分布变宽,耐环境应力开裂性能改善,加工性能优异。     

FCC催化剂用铝溶胶的制备及性能评价

采用添加适量铝粉的酸解-胶化工艺制备铝溶胶,采用pH计、旋转流变仪、纳米粒度与zeta电位仪等对铝溶胶的理化性质进行表征,用制得的铝溶胶样品制备成催化剂进行固定床反应评价。结果表明：采用添加适量铝粉的酸解-胶化工艺制得的铝溶胶氧化铝质量分数可达20%,氯质量分数不高于15%,pH为2.3,溶胶稳定性良好,可以满足FCC催化剂的实际使用要求。