scholarly journals Recrystallization and Micronization of p-Toluenesulfonamide Using the Rapid Expansion of Supercritical Solution (RESS) Process

Crystals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 449 ◽  
Author(s):  
Tsung-Mao Yang ◽  
Chie-Shaan Su ◽  
Jin-Shuh Li ◽  
Kai-Tai Lu ◽  
Tsao-Fa Yeh

This study is focused on the micronization of p-toluenesulfonamide (p-TSA) using the rapid expansion of supercritical solution (RESS) process. Taguchi’s experimental design method was applied to determine the optimum operating conditions. L9(34) orthogonal array with four control factors and three levels of each control factor was used to design nine experimental conditions. Four control factors were selected, including extraction temperature, extraction pressure, pre-expansion temperature, and post-expansion temperature. The particle size and morphology of the prepared samples were observed by scanning electron microscopy (SEM). In addition, Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC) were employed to compare the differences between the raw and micronized p-TSA particles. The experimental and analytical results indicated that the extraction temperature was the most significant factor for the micronization of p-TSA in the RESS process, and the optimal operating conditions were at an extraction temperature of 50 °C, an extraction pressure of 220 MPa, a pre-expansion temperature of 220 °C, and a post-expansion temperature of 30 °C. The p-TSA particles were micronized from the original average size of 294.8 μm to the smallest average size of 1.1 μm at the optimal RESS process conditions. Furthermore, the physicochemical characteristics of p-TSA did not differ significantly before and after recrystallization.

2020 ◽  
Vol 10 (2) ◽  
pp. 88-97
Author(s):  
Zafer Ekinci ◽  
Esref Kurdal ◽  
Meltem Kizilca Coruh

Background: Turkey is approximately 72% of the world’s boron sources. Colemanite, tincal, ulexite and pandermite are among the most significant in Turkey. Boron compounds and minerals are widely used in many industrial fields. Objective: The main purpose of this study was to investigate the control of impurities in the boric acid production process using colemanite by carrying out the reaction with a mixture of CO2 and SO2 - water, and determining the appropriate process conditions to develop a new process as an alternative to the use of sulfuric acid. Due to worrying environmental problems, intensive studies are being carried out globally to reduce the amount of CO2 and SO2 gases released to the atmosphere. Methods: The Taguchi method is an experimental design method that minimizes the product and process variability by selecting the most appropriate combination of the levels of controllable factors compared to uncontrollable factors. Results: It was evaluated the effects of parameters such as reaction temperature, solid-to liquid ratio, SO2/CO2 gas flow rate, particle size, stirring speed and reaction time. The optimum conditions determined to be reaction temperature of 45°C; a solid–liquid ratio of 0.083 g.mL−1; an SO2/CO2 ratio of 2/2 mL.s−1; a particle size of -0.354+0 .210 mm; a mixing speed of 750 rpm and a reaction time of 20 min. Conclusion: Under optimum operating conditions, 96.8% of colemanite was dissolved. It is thought that the industrial application of this study will have positive effects on the greenhouse effect by contributing to the reduction of CO2 and SO2 emissions that cause global warming.


2019 ◽  
Vol 8 (4) ◽  
pp. 6756-6760

Rapid expansion supercritical solution (RESS) is a technology introduced that produces a small solid oil particle with organic solvent free particle. RESS method is a better method compared to the traditional method due to many advantages such are produce clean extraction yields, obtain free solvent traces, environmental friendly and short processing time can be used in various industries such as cosmetic and pharmaceutical. Therefore, RESS technique is applied in order to produce direct solid oil particle from Luecaena leucocephala (L.leucocephala) pods instead of oil. In this study, the operating condition that applied during the RESS process in order to obtain the highest solid oil particle from the L.leucocephala pods sample are extraction temperature of 40 ºC, 45 ºC, 50 ºC, 55 ºC and 60 ºC and extraction pressure of 3000 psi, 4000 psi, 5000 psi, 6000 psi and 7000 psi at the constant extraction time of 40 minutes. The highest yield of L.leucocephala solid oil particles that obtained is about 0.65% at 60 oC and 7000 psi. The major components that obtained from the highest yield are 2,2,3-trimethyldecane, Cyclopentanone, propanoic acid and Cyclobutane, 1,2-diphenyl- by as identified by using Gas Chromatography Mass Spectrometry (GCMS).


2018 ◽  
Vol 8 (12) ◽  
pp. 2382
Author(s):  
Meng-Hua Li ◽  
Shen-Tsu Wang

In order to use touch control products more conveniently, a general objective is to develop lighter and smaller touch panels. A touch panel using the one glass solution (OGS) is an important development. The black matrix (BM) in an OGS touch panel is used as a black frame. The photoresist is divided into a positive photoresist and a negative photoresist. The BM photoresist is negative. After coating, exposure, and development in the BM process, after-develop inspection is implemented to check if the appearance is abnormal. It is quite difficult to rework the negative photoresist process. There is still room for improving the BM photoresist process capability Cpk. Thus, in order to reduce the customer complaint rate and enhance stability, the photolithography process is improved to enhance Cpk. Among the BM black negative photoresist forming process conditions of OGS products, the pre-baking time is the most important process control factor. The method set up herein improves the original Cpk = 0.90. This study employs the fast messy genetic algorithm (fmGA) to select the optimum orthogonal array of the Taguchi method, so as to implement the decision process of optimum parameter design. The Cpk of the optimum parameter is 2.12.


2021 ◽  
pp. 2150037
Author(s):  
Zahra Rezvanjoo ◽  
Farhad Raofie

Terminalia chebula pharmaceuticals were extracted by using the supercritical fluid extraction (SFE) technique. Under the optimal conditions of 184 [Formula: see text]L modifier volume, 46 min dynamic extraction time, and 316 atm fluid pressure, the extraction procedure was optimized by central composite design. A modified rapid expansion of supercritical solution (RESS) technique, named expansion of the supercritical solution (ESS) was used to create the extracted pharmaceutical nanoparticles (NPs). In ESS, supercritical carbon dioxide (SC-CO[Formula: see text] was saturated with the extracts at high-pressure. Next, a pressure drop reduced the SC-CO2 solubility power in a way the extracts started to precipitate. In contrast to RESS, the pressure was permanently conserved above the critical pressure before and after depressurization. Therefore, the expansion process was gentle, which led to obtaining small and uniform particles. In the NP production process, the most adequate parameters were 360[Formula: see text]atm premier pressure, 120[Formula: see text]atm subsequent pressure, 25[Formula: see text]min equilibrium time, 30[Formula: see text]min sedimentation time, and [Formula: see text]C temperature. The average size of precipitated NPs was 41[Formula: see text]nm according to the results of field emission scanning electron microscopy analysis. The liquid chromatography-mass spectrometry evaluation demonstrated the presence of chebulinic and chebulagic acids in the extracted sample.


ROTOR ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 13
Author(s):  
Mohammad Hartono ◽  
Hari Arbiantara Basuki ◽  
Andi Sanata

Quality of product in various industries, especially in metal industry is the most attention so the product can compete and attract consumers. Surface roughness is one of the demand that must be fulfilled because it can be the initiation of cracks, especially when material receives recurring and fluctuating loading. Therefore, low surface roughness can produce a product with longer lifespan material. The goal of this study is to determine the most optimal combination of electroplating process with factors variety of voltage (volts), temperature (℃), and time of immersion (minutes) to produce a low values of surface roughness. This study uses an experimental design with Taguchi method. Contribution factors of control that produce the surface roughness values ​​were influenced significantly by control factor voltage (volts) amounted to 77.31% with an average roughness value of 1.29 μm. This is due to the increase in voltage which causes the deposition of electrolyte ions which is faster in the deposition structure of the specimen. Where as other control factors were not effected significantly on the temperature control factor amounted to 4.85% with an average roughness value of 1,32 μm. These results are possible because the temperature variations used (40℃ to 50℃) are still within the optimum operating temperature. And the other control factors is immersion time amounted to 10.13% with an average roughness value of 1,32. The result ware obtained because the length of coating time affected the quantity of deposition of nickel ions on the surface of the specimen. The result of optimal condition is  the voltage level 2 (6 volts), the temperature at level 2 (45℃), and the immersion time at level 3 (25 minutes).


2016 ◽  
Vol 5 (2) ◽  
pp. 255
Author(s):  
Francesco Ferella ◽  
Ida De Michelis ◽  
Francesco Veglio

<p class="emsd-body"><span lang="EN-GB">Arsenic removal is hindered by its valence state. Addition of lime into wastewater containing arsenic gives benefits through the formation of low-soluble calcium arsenate, but the mechanism involved in the reduction of arsenic dissolution is not well known yet. Hence, in the present work different Ca/As ratios from 0 to 70% w/w were tested with the aim of finding the best conditions for removal of As from water (neutral tests) or solution (acid tests) containing sulphate ions. These solutions simulated aqueous streams coming from a wet scrubber for treatment of flue gas. Moreover, 5 g L<sup>-1</sup> of iron chloride were tested as additive in the acid tests. </span></p><p class="emsd-body"><span lang="EN-GB">In the optimum operating conditions, nearly 99% precipitation yield was obtained for both As(III) and As(V) in less than 1 h; the optimum process conditions were 10 g L<sup>-1</sup> of CaO without FeCl<sub>3</sub> for As(III) and 9 g L<sup>-1</sup> of CaO and 5 g <sup>-1</sup> FeCl<sub>3</sub> for As(V) in acid solutions. As regards neutral solutions, 1 g L<sup>-1</sup> of CaO is enough to precipitate around 99% of As(III) whereas the same result for As(V) is achieved by a higher CaO concentration (40 g L<sup>-1</sup>). Iron chloride had a negative effect on As(III) precipitation.</span></p>


Pharmaceutics ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 42 ◽  
Author(s):  
Yung-Tai Hsu ◽  
Chie-Shaan Su

In this study, the rapid expansion of the supercritical solutions (RESS) process was used to produce microparticles of a commonly used anti-inflammatory drug, ethenzamide. The effects of process parameters in RESS including the extraction temperature, pre-expansion temperature, and post-expansion temperature were investigated using the Box–Behnken design. According to the results of the analysis of variance (ANOVA), the effect of pre-expansion temperature is the most significant parameter on the mean size of RESS-produced ethenzamide. A higher pre-expansion temperature benefits the production of smaller crystals. In addition, a quadratic effect of the post-expansion temperature was also identified. Through RESS, ethenzamide microparticles with a mean size of 1.6 μm were successfully produced. The solid-state properties including the crystal habit, crystal form, thermal behavior, and spectrometric property were characterized by scanning electron microscopy (SEM), Fourier-transform infrared spectrometer (FTIR), differential scanning calorimeter (DSC), and powder X-ray diffraction (PXRD). These analytical results show that the rod-like crystals were generated through RESS, and the crystal form, thermal behavior, and spectrometric property of RESS-produced crystals are consistent with the unprocessed ethenzamide.


2012 ◽  
Vol 550-553 ◽  
pp. 1014-1025 ◽  
Author(s):  
Yong Bing Liu ◽  
Xing Wu ◽  
Yue Jin Liu ◽  
Jian Min Yi

To prepare ultra-fine particles and offer correlative applications such as the micronization of drugs with rapid expansion of supercritical solution (RESS), the first work in measuring the solubility of risocaine has been carried out at different operation conditions in this paper. The trend of solubility due to changes in specific operational parameters has been examined. The results of pressure (9-30 MPa) and temperature (308-328K) effecting on solubility show that the solubility increases mainly along with the increasing density. With applying different models to correlate the solubility data, we found Chrastil models had better correlation effects than the Peng Robinson EOS model, Mendez-Santiago and Teja equation model, with providing a nearly perfect average absolute relative deviation (AARD) of 0.0596. In the second part of work, RESS was applied to prepare risocaine particles at five different process conditions, including extraction temperature (308-328K), extraction pressure (9-30MPa), nozzle temperature (100-120°C), nozzle diameter (0.1-0.4nm) and spray distance (2-4cm).The size and morphology were determined by scanning electron microscopy (SEM). On the basis of the different experimental operation conditions, granular, filmily and threadlike particles with diameter (1-100nm) were obtained, it was also demonstrated that a successful size reduction of risocaine particles.


Author(s):  
Muhammad Ali Inam ◽  
Rizwan Khan ◽  
Kang-Hoon Lee ◽  
Young-Min Wie

The chronic ingestion of arsenic (As) contaminated water has raised significant health concerns worldwide. Iron-based coagulants have been widely used to remove As oxyanions from drinking water sources. In addition, the system’s ability to lower As within the maximum acceptable contamination level (MCL) is critical for protecting human health from its detrimental effects. Accordingly, the current study comprehensively investigates the performance of As removal under various influencing factors including pH, contact time, temperature, As (III, V) concentration, ferric chloride (FC) dose, and interfering ions. The optimum pH for As (V) removal with FC was found to be pH 6–7, and it gradually decreased as the pH increased. In contrast, As (III) removal increased with an increase in pH with an optimum pH range of 7–10. The adsorption of As on precipitated iron hydroxide (FHO) was better fitted with pseudo-second order and modified Langmuir–Freundlich models. The antagonistic effect of temperature on As removal with FC was observed, with optimum temperature of 15–25 °C. After critically evaluating the optimum operating conditions, the uptake indices of both As species were developed to select appropriate an FC dose for achieving the MCL level. The results show that the relationship between residual concentration, FC dose, and adsorption affinity of the system was well represented by uptake indices. The higher FC dose was required for suspensions containing greater concentration of As species to achieve MCL level. The As (V) species with a greater adsorption affinity towards FHO require a relatively smaller FC dose than As (III) ions. Moreover, the significant influence of interfering species on As removal was observed in simulated natural water. The author hopes that this study may help researchers and the drinking water industry to develop uptake indices of other targeted pollutants in achieving MCL level during water treatment operations in order to ensure public health safety.


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