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Investigation of the catalуtic activitу of K2CO3 in the carboxуlation reaction of phenol with sodium ethуl carbonate K2CO3在苯酚与碳酸钠羧化反应中的催化活性研究
IF 0.3 Pub Date : 2019-05-29 DOI: 10.15328/CB1061
K. A. Suerbaev, K. Shalmagambetov, G. Zhaksylykova, N. Kudaibergenov, M. Kozhakhmet
The catalуtic activitу of К2СО3 in the carboxуlation reaction of phenol with sodium ethуl carbonate has been investigated. The aim of the research was to develop a new efficient method for producing salicylic acid which is widely used in pharmaceuticals and other type preparations, also used in agriculture as an effective plant growth promoter. The most widespread synthesis method of salicylic acid is the Kolbe-Schmitt of phenol carboxylation, but it has a number of serious disadvantages. One of the alternative methods is the use of alkali metal salts of mono ethers of the carbonic acids as carboxylating agents in the carboxylation of phenol. In order to improve the method of production of salicylic acid, the catalytic activity of the К2СО3 catalyst at the carboxylation of phenol with sodium ethyl carbonate was studied for the first time. The effect of the process parameters (temperature, pressure, reaction time, ratio of catalyst to carboxylating agent) on the yield of the target product was studied. It was found optimal conditions: T=160°C, PCO2=10 atm, τ=7(4+3) h, [К2СО3]:[SEC]=0.07:1 at which the yield of the target product was 80%. The yields of the target product at phenol carboxylation with sodium ethyl carbonate in the presence and without K2CO3 were determined. It was found that К2СО3 shows the catalytic activity during carboxylation reaction.
研究了К2СО3在苯酚与碳酸钠的羰基化反应中的催化活性。这项研究的目的是开发一种新的高效生产水杨酸的方法,水杨酸被广泛用于制药和其他类型的制剂,也被用作有效的植物生长促进剂。水杨酸最广泛的合成方法是苯酚羧化的Kolbe-Schmitt法,但它有许多严重的缺点。替代方法之一是在苯酚的羧化中使用碳酸的单醚的碱金属盐作为羧化剂。为了改进水杨酸的生产方法,首次研究了К2СО3催化剂对苯酚与乙基碳酸钠羧化反应的催化活性。研究了工艺参数(温度、压力、反应时间、催化剂与羧化剂的比例)对目标产物收率的影响。确定了最佳条件:T=160°C,PCO2=10atm,τ=7(4+3)h,[К2СО3]:[SEC]=0.07:1,目标产物的产率为80%。测定了在K2CO3存在和不存在下用碳酸乙酯钠进行苯酚羧化时目标产物的产率。研究发现К2СО3在羧化反应中表现出催化活性。
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引用次数: 0
The study of fly ash filler behaviour in the polymer matrix of polyethyleneterephthalate 粉煤灰填料在聚对苯二甲酸乙二酯聚合物基体中的性能研究
IF 0.3 Pub Date : 2019-03-29 DOI: 10.15328/CB1018
T. Ketegenov, N. Khan, O. Tyumentseva, A. Karagulanova
The purpose of the investigation was to study the behavior of mechanically activated fly ash filler containing carbon in a polymer matrix of polyethylene terephthalate (PET). By means of the methods of optical and electron microscopy the change of physical and chemical properties of fly ash after intensive grinding in planetary mills of centrifugal type was considered. The research showed that mechanically activated filler, in contrast to its non-activated analog, structures the polymer matrix and provides improving the characteristics of the composite material.
研究了含碳机械活化粉煤灰填料在聚对苯二甲酸乙二醇酯(PET)聚合物基体中的性能。采用光学和电子显微镜等方法,研究了离心行星磨机对粉煤灰进行强磨后理化性质的变化。研究表明,与非活化的类似物相比,机械活化填料可以构造聚合物基体,并改善复合材料的特性。
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引用次数: 0
Concentration of uranium isotopes by in-situ coprecipitation on activated coal and iron (III) hydroxide 活化煤与氢氧化铁原位共沉淀法测定铀同位素浓度
IF 0.3 Pub Date : 2019-03-29 DOI: 10.15328/cb1000
I. Matveyeva, Fatima S. Meiirman, N. Nursapina, B. Satybaldiyev, T. Tuzova, Zh. Shalabayev, B. Shynybek
The use of the method of nonequilibrium uranium in various branches of science led to the necessity to determine its isotopic composition. The content of uranium isotopes in natural waters is often extremely low, therefore, it is necessary to collect significant volumes of samples in order to obtain reliable results of analysis. In this paper, it is proposed to concentrate uranium isotopes from water in-situ. Two alternative methods of uranium coprecipitation in field conditions (on activated carbon and iron (III) hydroxide) are considered. The desorbed uranium isotopes are determined by an alpha-spectrometric method with preliminary radiochemical preparation in laboratory conditions, including extraction with tributyl phosphate and electrodeposition on a steel disc. It was found that when concentrating on activated carbon the chemical yield was from 2 to 32%, and when concentrating on iron (III) hydroxide it is from 15 to 62%. For the second case, the chemical yield is acceptable for radiochemical work, and the proposed method for concentrating of uranium isotopes is recommended for usage in field conditions. Approbation of the method was carried out within the framework of the PEER454 project in 2017 in the valley of the river Ziddy, Pamir-Alay, Republic of Tajikistan. Work in the field conditions showed high efficiency of the method and its full feasibility even in the absence of acceptable laboratory conditions.
在不同的科学分支中使用非平衡铀的方法导致了确定其同位素组成的必要性。天然水体中铀同位素的含量往往极低,因此,为了获得可靠的分析结果,有必要收集大量样品。提出了从水中就地富集铀同位素的方法。考虑了现场条件下铀共沉淀的两种替代方法(活性炭和氢氧化铁)。解吸铀同位素用α光谱法测定,并在实验室条件下进行初步放射化学准备,包括用磷酸三丁酯萃取和在钢盘上电沉积。结果表明,浓缩活性炭的化学收率为2% ~ 32%,浓缩氢氧化铁的化学收率为15% ~ 62%。对于第二种情况,化学产量对于放射化学工作是可以接受的,建议在野外条件下使用拟议的铀同位素浓缩方法。该方法于2017年在塔吉克斯坦共和国帕米尔阿莱的齐迪河流域的PEER454项目框架内进行了批准。在现场条件下的工作表明,即使在没有可接受的实验室条件下,该方法也具有很高的效率和完全的可行性。
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引用次数: 0
The effect of mechanochemical activation and γ-radiation to a depth of coal catalytic hydrogenation of deposit Mamyt 机械化学活化和γ辐射对煤催化加氢深度的影响
IF 0.3 Pub Date : 2019-03-29 DOI: 10.15328/CB1041
Z. Kairbekov, S. Suimbayeva, I. Jeldybayeva, Murtezaoglu Kirali, Yelmira Yermoldina
This article presents the results of the mechanochemical activation of coal in a shock-grinding-type mill and the γ-radiation effect of a stream of electrons at the LU-6 electron accelerator. It was established that during the hydrogenation of dispersed coal, the yield of both total liquid products and coal distillates of various fractional composition increases. The maximum yield of liquid products (69.2 wt.%), gasoline (13.9 wt.%) and diesel (18.7 wt.%) fractions was observed during the hydrogenation of crushed coal for 30 min. It has been shown that the irradiation of coal with an electron flow (an irradiation dose of 150 kGy) also increases its reactivity in the process of hydrogenation, and also promotes the formation of free radicals and changes in iron compounds that make up the coal hydrogenation catalyst based on natural bauxite from the Turgai deposit. The non-linear regression method established the functional dependence of the yield of liquid products on the radiation dose, on the time of mechanical activation and on the concentration of free radicals, which are of an extreme nature.
本文介绍了煤在冲击磨机中机械化学活化的结果,以及在LU-6电子加速器中电子流的γ辐射效应。结果表明,在分散煤加氢过程中,总液体产物和各馏分煤馏分的产率均有提高。粉碎煤加氢30 min,液体产物(69.2 wt.%)、汽油馏分(13.9 wt.%)和柴油馏分(18.7 wt.%)收率最高。实验表明,在加氢过程中,电子流辐照(辐照剂量为150 kGy)也能提高煤的反应性。并促进自由基的形成和铁化合物的变化,这些铁化合物构成了煤加氢催化剂,这些催化剂基于图尔盖矿床的天然铝土矿。非线性回归方法建立了液产物产率与辐射剂量、机械活化时间和自由基浓度的函数依赖关系。
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引用次数: 0
Sorption of lead and cadmium ions from aqueous solutions using modified zeolite 改性沸石对水溶液中铅和镉离子的吸附
IF 0.3 Pub Date : 2018-12-28 DOI: 10.15328/cb980
M. Telkhozhayeva, G. Seilkhanova, A. Rakhym, A. Imangaliyeva, D. Akbayeva
The processes of lead and cadmium ions sorption by modified zeolite of Chankanai deposit were studied. Chitosan was used as a surface modifier due to its properties: nontoxicity, biodegradability and biocompatibility. The adsorption process was carried out at room temperature (295 K) and pH 7 under static conditions. The synthesized sorbent has been characterized by scanning electron microscopy (SEM), elemental analysis; the concentrations of Pb(II) and Cd(II) ions before and after adsorption were determined using atomic absorption spectroscopy (AAS). The Si/Al ratio of the zeolite was found to be 1.66, which showed the prospects of using this material as a source object. The static exchange capacity (SEC) of sorbents and the extraction degree of heavy metal ions were determined and compared. It was found that the removal of heavy metal ions increased with the increase of contact time (removal efficiency was 99.1±1.2% for Pb2+ and 83.4±1.2% for Cd2+). The adsorption capacity values of the modified zeolite for metal ions were (0.86±0.03) mg/g for Cd(II) and (0.68±0.03) mg/g for Pb(II). Chitosan-modified zeolite proved to be an effective adsorbent for removal of lead and cadmium ions from aqueous solutions.
研究了Chankanai矿床改性沸石吸附铅、镉离子的过程。壳聚糖具有无毒、可生物降解和生物相容性等特点,被用作表面改性剂。吸附过程在室温(295 K)和pH为7的静态条件下进行。通过扫描电镜(SEM)、元素分析对合成的吸附剂进行了表征;采用原子吸收光谱法(AAS)测定吸附前后Pb(II)和Cd(II)离子的浓度。该分子筛的Si/Al比值为1.66,显示了该材料作为源物的前景。测定并比较了吸附剂的静态交换容量和对重金属离子的萃取程度。结果表明,随着接触时间的增加,对重金属离子的去除率提高(Pb2+去除率为99.1±1.2%,Cd2+去除率为83.4±1.2%)。改性沸石对金属离子的吸附量分别为Cd(II)(0.86±0.03)mg/g和Pb(II)(0.68±0.03)mg/g。壳聚糖改性沸石是一种去除水中铅和镉离子的有效吸附剂。
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引用次数: 3
Synthesis and identification of 3,5-bis(hydroxymethyl)tetrahydro-4H-pyran-4-one 3,5-双(羟甲基)四氢-4H-吡喃-4-酮的合成与鉴定
IF 0.3 Pub Date : 2018-12-28 DOI: 10.15328/CB1039
K. Bazhykova, P. Langer, E. Yergaliyeva, Tulegen M. Seylkhanov, Z. Abilov
3,5-bis(hydroxymethyl)tetrahydro-4H-pyran-4-one by condensation of acetone with formaldehyde in the ratio of 1:4 in an alkaline medium at a temperature of 30-35°С (product yield 67.4%) was obtained. To determine the composition of obtained compound elemental analysis was used. Functional composition and structural elements were identified using IR spectroscopy. To prove the structure of the synthesized compound, 1H and 13C NMR spectra were taken on a JNN-ECA Jeol 400 spectrometer (at a frequency of 399.78 MHz and 100.53 MHz) with a CDCl3 solvent. Quantum-chemical calculations of stable conformations of 3,5-bis(hydroxymethyl)tetrahydro-4H-pyran-4-one was performed using ab initio DFT B3LYP method and 6-31G (d) and 6-311+G(3df,2p) basis sets. It was found that the stable conformers obtained by calculations are in the "chair" conformation; the hydroxymethyl substituents in conformer I are located equatorially, in conformation II – axially and equatorially, in conformation III – axially. In the conformer III, as a result of spatial proximity, hydroxymethyl substituents form an intramolecular hydrogen bond. The total energies and dipole moments were calculated; a lower value of the dipole moment of the conformation II may indicate its preference over the others.
丙酮与甲醛在30-35°С碱性介质中以1:4的比例缩合得到3,5-双(羟甲基)四氢- 4h -吡喃-4- 1,产物收率为67.4%。用元素分析法测定所得化合物的组成。用红外光谱法鉴定了其功能成分和结构元素。为了证明合成化合物的结构,以CDCl3为溶剂,在JNN-ECA Jeol 400光谱仪(频率分别为399.78 MHz和100.53 MHz)上进行1H和13C NMR谱分析。采用从头算DFT B3LYP方法和6-31G (d)和6-311+G(3df,2p)基集对3,5-双(羟甲基)四氢- 4h -吡喃-4-one的稳定构象进行了量子化学计算。计算得到的稳定构象为“椅子”构象;构象I中的羟基甲基取代基在轴向的构象II和轴向的构象I中均位于赤道上。在构象III中,由于空间接近,羟甲基取代基形成分子内氢键。计算了总能量和偶极矩;偶极矩值较低的构象II可能表明其优于其他构象。
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引用次数: 2
Исследование эксплуатационных характеристик дорожного битума, модифицированного отходами полиэтилена 聚乙烯废物改良沥青路性能研究
IF 0.3 Pub Date : 2018-12-28 DOI: 10.15328/cb1028
S. S. Satayeva, Aibarsha G. Аbdrakhmanova, Anar S. Kurmangaliyeva
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引用次数: 1
Study of effectiveness of strongly basic anion exchange resins in the process of uranium extraction from the underground leaching productive solution 强碱性阴离子交换树脂在地下浸出生产液提铀过程中的有效性研究
IF 0.3 Pub Date : 2018-12-28 DOI: 10.15328/CB979
N. Nursapina, Fatima S. Meiirman, G. Amanova, I. Matveyeva
The process of uranium sorption is one of the important stages in the production of uranium. This stage affects uranium extraction effectiveness from productive solutions. The sorption and desorption characteristic of anion exchange resins in dynamic condition were investigated in order to study the effectiveness of resins, which were used for extraction of uranium from sulfuric acid productive solution. The sorption and desorption of uranium from the productive solution on anion exchange resins AB-17 and DOWEX 1X8 200 was carried out in laboratory conditions. The sorption characteristics were investigated. The determined sorption capacities of the resins were 1.47 and 14.4 mg/mL, respectively. The most efficient anion exchanger is DOWEX 1X8 200 that has a high sorption capacity as well as good desorption characteristics, which make it possible to obtain solutions having 23 times higher uranium concentrations than in productive solutions.
铀的吸附过程是铀生产的重要阶段之一。这一阶段影响从生产性溶液中提取铀的有效性。研究了阴离子交换树脂在动态条件下的吸附和解吸特性,以研究该树脂用于从硫酸生产溶液中提取铀的有效性。在实验室条件下,用阴离子交换树脂AB-17和DOWEX1X8200对生产溶液中的铀进行了吸附和解吸。研究了吸附特性。所测定的树脂的吸附容量分别为1.47和14.4mg/mL。最有效的阴离子交换剂是DOWEX 1X8 200,它具有高吸附能力和良好的解吸特性,这使得获得铀浓度比生产溶液高23倍的溶液成为可能。
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引用次数: 1
Self-propagating high-temperature synthesis of refractory powder materials based on zirconium diboride obtained from boron-containing mineral raw materials of the Republic of Kazakhstan 以哈萨克斯坦含硼矿物原料为原料制备的二硼化锆耐火粉末材料的自蔓延高温合成
IF 0.3 Pub Date : 2018-09-29 DOI: 10.15328/cb982
A. Batkal, Gulnaz K. Temirlanova, Elaman M. Satybaldiyev, Aizhan Zh. Seydualieva, R. Abdulkarimova
The goal of the present work is the synthesis of the refractory zirconium diboride powder in the combustion mode. One of the most effective methods of synthesis of the refractory zirconium diboride powder is the self-propagating high-temperature synthesis method (SHS) with a preliminary mechanical activation of the initial components. Initial components of the SH-synthesis are borate ore, zircon, aluminum powder and magnesium. After the SH-synthesis obtained products were processed by 37.5% HCl and were washed with distilled water. Final composition and microstructure of SHS products were investigated with X-ray phase analysis and SEM. Boron-containing SHS-powders can be used as bio-protection in nuclear engineering, production of abrasive powders, ceramic, composite materials and coatings.
本工作的目标是在燃烧模式下合成耐火的二硼化锆粉末。合成难熔二硼化锆粉末的最有效方法之一是对初始组分进行初步机械活化的自蔓延高温合成法(SHS)。SH合成的初始成分是硼酸盐矿石、锆石、铝粉和镁。SH合成后,用37.5%HCl处理得到的产物,并用蒸馏水洗涤。用X射线相分析和扫描电镜研究了SHS产物的最终组成和微观结构。含硼SHS粉末可用于核工程、磨料粉末生产、陶瓷、复合材料和涂层的生物防护。
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引用次数: 1
Hydrothermal synthesis of monostructured LaPO4: morphology and structure 单结构LaPO4的水热合成:形貌和结构
IF 0.3 Pub Date : 2018-09-29 DOI: 10.15328/cb1015
K. Kenges, M. Aldabergenov, O. Proskurina, V. Gusarov
The application field of materials based on lanthanum orthophosphate (LaPO4) including nanomaterials, has been permanently extending recently. The high level of mechanical properties and the compatibility with numerous oxides make it possible to consider the possibility of using lanthanum orthophosphate as a composite material for construction purposes. This application is particularly promising when nanoparticles with quasi-1D morphology (nanorods) are used. The high isomorphic capacity of the LaPO4-based phase for alkaline-earth ions and ions of lanthanides and actinides, high chemical stability, and high radiation hardness make promising the application of this compound as a matrix for immobilization of radioactive wastes. The possibility of obtaining lanthanum phosphate (LaPO4) by the hydrothermal method is considered in the work. Effects of pH, temperature and time of processing of hydrothermal synthesis on the morphology and structure of monostructured lanthanum phosphate are studied. It has been established that, with the increase of pH, the morphology of phosphate changed, the size of the crystallites increased, while the crystal structure changed from hexagonal to monoclinic.
基于正磷酸镧(LaPO4)的材料(包括纳米材料)的应用领域近年来得到了永久性的扩展。高水平的机械性能和与多种氧化物的兼容性使得考虑使用正磷酸镧作为复合材料用于建筑目的的可能性成为可能。当使用具有准1D形态的纳米颗粒(纳米棒)时,这种应用特别有前景。LaPO4基相对碱土离子以及镧系元素和锕系元素离子的高同构能力、高化学稳定性和高辐射硬度使该化合物有望作为固定放射性废物的基质应用。考虑了水热法合成磷酸镧(LaPO4)的可能性。研究了水热合成过程中pH、温度和时间对磷酸镧单结构形貌和结构的影响。研究表明,随着pH的增加,磷酸盐的形态发生了变化,晶粒尺寸增大,晶体结构由六方晶系变为单斜晶系。
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引用次数: 1
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Chemical Bulletin of Kazakh National University
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