Novel Process For Preparation Research Articles

Fabrication of TiB2 coatings by electrophoretic deposition of synthesized TiB2 nanoparticles in molten salts

This paper presents a novel process for preparation of TiB2 coatings, which is a combination of synthesis of TiB2 nanoparticles by borothermal reduction of TiO2 in molten NaCl–KCl–AlF3 system and subsequent electrophoretic deposition of the as-synthesized TiB2 nanoparticles in the same molten salts system. The electrophoretic deposition under various cell voltages was carried out, which resulted in preparation of dense and relatively flat TiB2 coatings. The effect of applied cell voltages on the electrophoretic deposition rate and mechanical properties of produced TiB2 coatings has been presented. The thickness of the coatings increased with the rise of cell voltages due to elevated migration and deposition rate of TiB2 nanoparticles. The hardness of the fabricated TiB2 coatings was assessed by nanoindentation, indicating that the values of hardness and elastic modulus increased with elevated electrophoretic voltages, which probably has an influence on the structure of the TiB2 coatings. Under the cell voltage of 1.2 V, the values of hardness and elastic modulus could reach 32.4 ± 1.2 GPa and 420.2 ± 23.9 GPa, respectively. This proposed process should also be applied for preparation of additional types of transition metal diboride coatings.

Optimization of a novel process for preparation of silicon carbide foams

Silicon carbide (SiC) was mixed with alumina and kaolin to obtain porous alumino-silicate bonded SiC specimens. These mixtures contain 40 to 80 mass% SiC while the alumina contents of their bonding materials are 60–80 mass%.Porous SiC specimens were prepared from mixtures of silicon carbide, calcined alumina and Klabsha kaolin using the foaming method. The employed technique of foaming introduces pores into SiC specimens as a result of chemical reaction between aluminum powder (Al) and calcium carbide (CaC2) in presence of water which liberates acetylene and hydrogen gases. The reaction and process are assisted by adding sodium meta-silicate and a stabilizer. The shaped specimens were dried and then fired up to 1450 °C for 2hrs.The chemical composition and firing temperature of foamed specimens are responsible for all changes occurring in their physical properties, microstructure characteristics and mineral composition.The result indicated that CaC2 mass% and CaC2/Al mass ratio of 1 and 3.3 are considered to be more suitable amounts for using in this foaming method and firing temperature as low as 1350 °C is used to prepare more porous specimens. Also on increasing the water content from 25 to 30 mass%, specimens of higher open porosities and lower bulk densities are obtained. Under these conditions, porous SiC specimens having bulk density, open porosity and mean pore size of 0.88–1 g/cm3, 65–70% and less than 25 μm are obtained, respectively.

Novel process for preparation of metal-polymer composite membranes for hydrogen separation

In the present work, a new preparation method for metal-polymer composite materials for hydrogen separation which consist of hydride-forming intermetallic compound LaNi5 and polyethylene was developed. According to this technique, the mechanical activation of the initial powder mixtures was employed to provide good interface between the phases. A series of composite membranes with various filler concentrations was synthesized and characterized by X-ray diffraction, scanning electron microscopy and differential scanning calorimetry. The gas transport properties of the obtained materials in relation to H2, O2, N2, CO2 and CH4 were tested. The results indicate that the addition of the hydride-forming intermetallic compound to the barrier polymer leads to significantly improved selectivity with respect to hydrogen. The proposed method can be considered as a promising approach to producing of high performance composite membranes for hydrogen separation.

Novel Process for Preparation of Tetrabenazine and Deutetrabenazine

The present invention provides process for preparation of dihydroxy benzoquinoline compound (III) comprising reacting dihydroxy isoquinoline compound (IV) or a salt thereof with (2-acetyl-4-methyl-pentyl)-trimethyl-ammonium iodide (V) and further 5 converting it to tetrabenazine (I) and deutetrabenazine (II).

A novel process for preparation of titanium dioxide from Ti-bearing electric furnace slag: NH4HF2-HF leaching and hydrolyzing process

A novel process to prepare titanium dioxide from Ti-bearing electric furnace slag by NH4HF2-HF leaching and hydrolyzing process has been developed. In this present study, the effects of [NH4+]/[F] mXolar ratio, leaching temperature, [F] concentration, liquid/solid mass ratio, leaching time on the Ti extraction, and the phase transformations have been investigated to reveal the leaching mechanism of Ti-bearing electric furnace slag in NH4HF2-HF solution. In the NH4HF2-HF leaching process, the MgTi2O5 and Al2TiO5 are converted to TiF62− and Mg-Al-bearing precipitate. Ti extraction rate reached 98.84% under the optimal conditions. In addition, 98.25% iron ions can be removed in the presence of NaCl prior to hydrolysis process. The effects of pH and temperature on the selective hydrolysis of TiF62− during hydrolysis process were also studied. In the hydrolysis process, the TiF62− is converted to (NH4)2TiOF4. By calcination, high grade TiO2 powder with its purity of 99.88% was obtained, using which the products, well crystallized anatase and rutile, were obtained through roasting at 800°C and 1000°C, respectively.

Combined production of synthetic rutile in the sulfate TiO2 process

Abstract This paper describes a novel process for preparation of synthetic rutile using an intermediate, sulfated ilmenite from the sulfate TiO 2 process as the feedstock. The synthetic rutile can be obtained by selective thermal decomposition of the sulfated ilmenite, followed by targeted leaching for removal of various impurities. The results of the decomposition unit showed that almost all the TiOSO 4 in the sulfated ilmenite decomposed to TiO 2 , while the iron component mainly existed in the form of sulfates in the optimal thermal decomposition conditions, i.e., a roasting temperature of 540 ° C and a roasting time of 120 min under air flow or in stagnant air or a roasting temperature of 510 ° C and a roasting time of 120 min under nitrogen flow. The thermal decomposition can be divided into three stages. The sulfates of titanium and iron in the sulfated ilmenite were first decomposed to TiO 2 and water-insoluble FeOHSO 4 , respectively, at a temperature less than 500 ° C. The FeOHSO 4 was further converted into water-soluble Fe 2 O(SO 4 ) 2 at 500–560 ° C. Finally, the Fe 2 O(SO 4 ) 2 was decomposed to Fe 2 (SO 4 ) 3 and Fe 2 O 3 at a temperature above 560 ° C. The water-soluble metal sulfates, the water-insoluble FeOHSO 4 /Fe 2 O 3 and the SiO 2 in the TiO 2 -containing slag can be removed through leaching by using water, dilute sulfuric acid and sodium hydroxide, respectively. The results showed that 70–85% of the iron, as well as a majority of the magnesium, calcium, etc. impurities, could be leached by water, and up to 92% of the total iron could be removed after the subsequent acid leaching in a 15 wt% H 2 SO 4 solution, while the silicon removal reached 65% in a 5 wt% NaOH solution. A synthetic rutile with a TiO 2 content over 90 wt% and total MgO + CaO less than 1 wt% was obtained under the optimal conditions listed above. The present process can be integrated with the sulfate TiO 2 process, producing titania pigment and synthetic rutile simultaneously. The advantages of the TiO 2 beneficiation process include the moderate reaction conditions, the capability of recycling the H 2 SO 4 completely and the recovery of a large part of the iron, as well as comprehensive utilization of the waste sulfuric acid discharged from the sulfate TiO 2 production process.

A novel process for preparation of fatty acid oil mixture in solid form.

The present study describes a novel and scalable process for preparation of omega-3 and omega-6 fatty acids in solid form. The process involves multiple steps consisting of combining the oil with a metal base in alcohol to form a solution, followed by addition of reaction mixture to acetonitrile (anti-solvent) to form a slurry and further separating the solid through filtration. This process results in formation of a flowable solid with yield of 44-76% depending on the procedure employed. The fatty acid profile of the calcium and magnesium salts was stable after one year of storage in ambient conditions. The type of solvent and anti-solvent employed in such process has tremendous effect on the resulting solid texture, which could range from complete gum to a workable, filterable solid. It was also demonstrated that increasing the concentration of base in alcohol reduces the amount of residual acetonitrile in the solid.

A novel process for preparation of hybrid nanosized neodymium oxybromide and neodymium oxide

A novel process to prepare hybrid nanosized neodymium oxybromide and neodymium oxide from neodymium(III) nitrate hexahydrate has been developed. The simultaneous use of two capping agents (cytosine and cetyltrimethylammonium bromide) in the process allows for efficient control of properties of the so synthesized nanoparticles. The product has been characterized by means of X-ray diffraction, infrared spectroscopy, field emission scanning electron microscopy, differential scanning calorimetry, and thermogravimetric analysis. The nanoparticles size ranges from 17.0 to 64.2 nm.

A Novel Process for Antimalarial Drug Pyronaridine Tetraphosphate

A novel process for preparation of pyronaridine tetraphosphate, an antimalarial drug substance, is reported. The overall yields are 54% and >99.8% (including five chemical steps). Formation and control of possible impurities are also described.

A Novel Process for Preparation of Unsupported Mesoporous Intermetallic NiZn and PdZn Catalysts

Unsupported mesoporous intermetallic (usmpIM) NiZn and PdZn catalysts are successfully prepared by means of a two-step procedure: (1) leaching of Al-based intermetallic compounds (Al3Ni, Al21Pd8) with 20 wt% NaOH aqueous solution and (2) immersion of ZnCl2 aqueous solution into unsupported porous Ni or Pd followed by alloying treatment under H2 flow at 500 °C, i.e., immersion alloying process. Thermal stability of the mesoporous structures is found to be improved by alloying with Zn. The catalytic properties for steam reforming of methanol (SRM) were completely different from the original unsupported porous Ni and Pd, where the decomposition of methanol and the SRM occurred preferentially on usmpIM NiZn and usmpIM PdZn, respectively.

A novel process for preparation of an ultra-clean superfine coal–oil slurry

A novel process for the preparation of an ultra-clean superfine coal–oil slurry is presented. The process uses a high-pressure water-jet mill and a pumping slurry jet mill for coal superfine comminution. The mean diameter of coal particles in the slurry is 2.71μm, and the ash content is 1.05%. The stability, rheological behavior, and heat value of the slurry are investigated. The results show that the ultra-clean superfine coal–oil slurry has a high heat value, a high level of stability, and low viscosity. The slurry can be used as fuel in a high-speed diesel engine. The total energy consumption of comminution of the coal particles to reduce the mean diameter from 3mm to about 2.71μm is 124kWh per ton, which is lower than the total energy consumption by traditional ball mills by about 50–70%.

A novel process for preparation of ultra-clean micronized coal by high pressure water jet comminution technique

A novel process for the preparation of ultra-clean micronized coal is presented in this paper. High pressure water jet mill replacing the ball mill is employed for coal comminution in the new preparation process, which is the essential difference from the traditional one. To compare the new preparation process with the traditional one, the comparison experiments were performed, with froth flotation tests of the fine particles ground by both mills using 0# diesel oil and n-dodecane as collector, 2-octanol as frother, and sink–float separation tests using mixtures of carbon tetrachloride–benzene and carbon tetrachloride–bromoform as dense liquid. Different parameters including combustible recovery, ash content of the clean coal, separation efficiency, and energy consumption were investigated based on the two different preparation processes. The results show that the new preparation process has high combustible recovery, low ash content of the product, high separation efficiency, and low energy consumption compared with the traditional one. The comminution mechanism of high pressure water jet mill is introduced in this paper. The high pressure water jet comminution technique has great potential in coal pulverization, having the advantages of low energy consumption, low iron content, and low equipment wear.

Unexpected Formation of Bicyclic Cyclopropane Lactam and Pyridone from the Reaction of cis‐2‐Aryl‐1‐carbomethoxy‐3,3‐dicynocyclopropane with Primary Aliphatic Amine via Isomerization and Rearrangement

The novel process for preparation of fused bicyclic cyclopropane lactams and multisubstituted pyridones was described. It is the first example of a successful isomerization and rearrangement of the cis‐cyclopropane with primary aliphatic amine.

A novel process for preparation of (1→3)-β- d-glucan sulphate by a heterogeneous reaction and its structural elucidation

(1→3)-β- d-Glucans have received increasing attentions with respect to their biological functions. Previously, a method combining cellular induced autolysis with subsequent oxidation by sodium hypochlorite to prepare (1→3)-β- d-glucan from Saccharomyces cerevisiae was developed. However, the poor aqueous solubility of the resultant polysaccharide was a huge hindrance to its application especially in pharmaceuticals. Herein, a novel glucan sulphation process, also a heterogeneous reaction system, composed of sulfuric acid and n-propanol with a molar ratio of 1.4, is proposed to improve polysaccharide polarity and its aqueous solubility. After the heterogeneous sulphation at −6 °C for 90 min, (1→3)-β- d-glucan sulphate yield was about 37.4% (w/w), the degree of sulphation 0.36, and its empirical formula was (C 6H 10O 5) 25·9SO 3·7H 2O according to elemental analysis. In addition, sulphation made the polysaccharide morphologically loosened according to observation under scanning electron microscopy. The presence of characteristic absorptions at 1246 and 813 cm −1 in the FTIR spectrum, as well as the 1H NMR spectrum demonstrated that the material was a sulphate ester of glucan.

99/00101 A novel process for preparation of active carbon from sapropelitic coals

The coal of the Miocene Bukit Asam deposit in south Sumatra is mostly sub-bituminous in rank, consistent with regional trends due to burial processes. However, effects associated with Plio–Pleistocene igneous intrusions have produced coal with vitrinite reflectance up to at least 4.17% (anthracite) in different parts of the deposit. The un-metamorphosed to slightly metamorphosed coals, with Rvmax values of 0.45–0.65%, contain a mineral assemblage made up almost entirely of well-ordered kaolinite and quartz. The more strongly heat-affected coals, with Rvmax values of more than 1.0%, are dominated by irregularly and regularly interstratified illite/smectite, poorly crystallized kaolinite and paragonite (Na mica), with chlorite in some of the anthracite materials. Kaolinite is abundant in the partings of the lower-rank coals, but is absent from the partings in the higher-rank areas, even at similar horizons in the same coal seam. Regularly interstratified illite/smectite, which is totally absent from the partings in the lower-rank coals, dominates the mineralogy in the partings associated with the higher-rank coal beds. A number of reactions involving the alteration of silicate minerals appear to have occurred in both the coal and the associated non-coal lithologies during the thermal metamorphism generated by the intrusions. The most prominent involve the disappearance of kaolinite, the appearance of irregularly interstratified illite/smectite, and the formation of regular I/S, paragonite and chlorite. Although regular I/S is identified in all of the non-coal partings associated with the higher-rank coals, illite/smectite with an ordered structure is only recognised in the coal samples collected from near the bases of the seams. The I/S in the coal samples adjacent to the floor of the highest rank seam also appears to have a greater proportion of illitic components. The availability of sodium and other non-mineral inorganic elements in the original coal to interact with the kaolinite, under different thermal and geochemical conditions, appears to be the significant factor in the formation of these new minerals, and distinguishes the mineralogical changes at Bukit Asam from those developed more generally with rank increases due to burial, and from the effects of intrusions into coals that were already at higher rank levels.

99/00136 A novel process for preparation of active carbon from sapropelitic coals

99/00136 A novel process for preparation of active carbon from sapropelitic coals

A novel process for preparation of active carbon from sapropelitic coals

The aim of this work is the preparation of active carbons starting from sapropelitic coals. Firstly, a traditional route of manufacturing, coking and activation (820°C) was carried out. The specific area (BET) of the activated semicokes of six sapropelitic coal samples varied from a few square meters to about five hundred (for Taimylir coal). Secondly, using Taimylir coal, a novel way of active carbon preparation was attempted combining low temperature modification and chemical activation. The modification was carried out using nitric acid-acetic anhydride mixture at room temperature and tested by swelling and weight uptake measurements. The modified coal samples were analyzed by Thermogravimetry (TGA) and FT-IR spectroscopy. The chemical activation route included impregnation by an activant (KOH) and a subsequent heating (2 hr under argon) at selected temperatures ranging from 300 to 900°C. Surface areas were determined by BET and SAXS methods. The chemical modification resulted in new functional group formation and organic framework reorganization, which strongly affected the activation, as a value of 1200 m 2 g −1 was obtained after chemical activation.

Electrical and mechanical properties of pre‐localized polypyrrole/poly(vinyl chloride) conductive composites

AbstractA novel process for preparation of conductive polypyrrole/poly(vinyl chloride) (PPy/PVC) composites by pre‐localization of an intrinsically conducting PPy phase in a PVC matrix has been developed. This process involves encapsulating PVC particles with a thin layer of PPy, and subsequently compacting this PPy‐encapsulated PVC powder by compression molding. The current‐voltage characteristics and electrical conductivity of the pre‐localized PPy/PVC composites were determined. The change of the current‐voltage characteristics from linear to nonlinear behavior with increasing PPy content in the composites is discussed in the view of the intermolecular hopping and tunneling of electrons. The tensile properties, dynamic mechanical behavior, and microhardness of the pre‐localized PPy/PVC composites were studied as a function of PPy content. A percolation threshold of 0.3 wt% is achieved in the pre‐localized PPy/PVC composites. This value is much lower than those of the conventional conductive composite materials containing a random distribution of PPy fillers. The samples with a PPy content of 1.6 wt% or above have high conductivity and still preserve reasonable mechanical properties.

ChemInform Abstract: A Novel Process for Preparation of a Cu/ZnO/Al2O3 Ultrafine Catalyst for Methanol Synthesis from CO2 + H2: Comparison of Various Preparation Methods.

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.

A novel process for preparation of a Cu/ZnO/Al 2O 3 ultrafine catalyst for methanol synthesis from CO 2 + H 2: comparison of various preparation methods

The effect of preparation methods on the structure and catalytic behavior of Cu/ZnO/Al 2O 3 catalysts for methanol synthesis from hydrogenation of carbon dioxide has been studied. The Cu/ZnO/Al 2O 3 ultrafine catalysts obtained by a novel gel-coprecipitation process exhibited higher catalytic activity for the synthesis of methanol from CO 2 + H 2. The results showed that isomorphous substitution took place between copper and zinc in the precipitates prepared by the novel process. Preparation methods have a significant influence on the structure of the catalyst and catalytic activity for methanol synthesis from hydrogenation of carbon dioxide.