Discrepancy between thermodynamic and kinetic stabilities of thetert-butanol hydrates and its implication for obtaining pharmaceutical powders by freeze-drying

2019 ◽  
Vol 55 (29) ◽  
pp. 4262-4265 ◽  
Author(s):  
A. G. Ogienko ◽  
A. S. Stoporev ◽  
A. A. Ogienko ◽  
M. S. Mel’gunov ◽  
T. P. Adamova ◽  
...  

The substitution of sublimed “H1 + Ih” for “H2 + Ih” leads to both a reduction of primary drying time and a significant increase in specific surface area of the trehalose freeze-dried cakes.

2021 ◽  
Vol 9 ◽  
pp. 68-78
Author(s):  
T. S. Kuznetsova ◽  
◽  
I. V. Burakova ◽  
T. V. Pasko ◽  
A. E. Burakov ◽  
...  

The paper presents a technique for obtaining a universal composite nanomaterial for effective sorption water purification from pollutants of various chemical nature. The proposed material is a nanocomposite based on reduced graphene oxide modified with a functional organic component — polyaniline, which also includes oxidized carbon nanotubes as a structure former. The use of polyaniline makes it possible to significantly increase the activity and sorption capacity of the developed graphene material. The authors were developed a number of nanocomposites, which differ in the final stage of the pre-prepared hydrogel technology: drying in air (drying oven), freeze drying, drying under supercritical conditions (supercritical fluid — isopropyl alcohol). In addition, the effect of carbonization as an additional stage (T = 800 °C, argon) was studied in the article. The materials surface morphology was evaluated using scanning electron microscopy. The specific surface area and the parameters of the porous space were determined by nitrogen adsorption. The materials specific surface area increases depending on the choice of drying technology for the initial hydrogel (drying oven — 80 m2/g → freeze drying — 180 m2/g → supercritical drying — 290 m2/g), and also increases after the carbonization stage and reaches a value of ~ 350 m2/g. The nanocomposites sorption capacity to the organic dyes (methylene blue (MB) and solar yellow (SY)), as well as to heavy metals (for example, zinc ions) was determined. It was found that the value of MB sorption is up 1380 to 1800 mg/g, for SY — up 159 to 300 mg/g, for zinc — up 31 to 230 mg/g. At the same time, the sample processed under supercritical conditions, followed by carbonization, were shown the best characteristics.


2018 ◽  
Vol 14 (7-8) ◽  
Author(s):  
Qing Xu ◽  
Yan Yao ◽  
Tong Zhao ◽  
Qiongqiong Shi ◽  
Zhanyong Li ◽  
...  

AbstractPullulan particles were prepared to improve water solubility. The pullulan droplet with the concentration of 5%, 10%, 15% or 20% (w/w) was injected and frozen in the cryogenic media of liquid nitrogen at −196 °C or cold air at −15 °C, then freeze dried. The results show that most of dried pullulan particles pre-processed in either liquid nitrogen or cold air can be completely dissolved in water within 60 s. The water solubility of as-prepared particles in liquid nitrogen is better than that in cold air. The particles frozen at −196 °C have smaller and more uniform pore structures together with a larger specific surface area than those frozen at −15 °C. It is found that the particles from 10% pullulan solution with liquid nitrogen have largest water solubility and also highest specific surface area (11.78 m2/g).


2020 ◽  
Vol 205 ◽  
pp. 09005
Author(s):  
Seyed Morteza Zeinali ◽  
Sherif L. Abdelaziz

Robust engineering of geomaterials for energy applications requires a clear understanding of the impacts of temperatures and pressures applied to the soil on their microstructures. Such understandings will facilitate better designs of new geomaterials and technologies via ensuring accurate assessments of the performance of the existing ones. In this study, we assess the changes in the microstructure—specific surface area and pore size distribution—of a saturated clay subjected to stress and temperature cycle. Clay specimens were subjected to the desired mechanical stresses and thermal cycles in a triaxial system. Then, the specimens were swiftly extracted from the triaxial, flush frozen in liquid nitrogen, then freeze-dried to preserve their microstructure. The preserved specimens were then used for specific surface area and pore size distribution assessments using nitrogen (N2)-gas adsorption and mercury intrusion porosimetry. The results established qualitative explanations of the expected microstructural changes in geomaterials under operational conditions, which facilitate the development of new geomaterials that can overcome such alternations.


2021 ◽  
Vol 71 (1) ◽  
pp. 81-98
Author(s):  
Maja Preskar ◽  
Danijel Videc ◽  
Franc Vrečer ◽  
Mirjana Gašperlin

AbstractThis study explores the use of a statistical model to build a design space for freeze-drying two formulations with ibuprofen. A 2 × 3 factorial experimental design was used to evaluate independent variables (filling volume and annealing time) and responses as residual moisture content, specific surface area and reconstitution time. A statistical model and response surface plots were generated to define the interactions among the selected variables. The models constructed for both formulations suggest that 1 mL of filled volume and no annealing should be used to achieve optimal residual moisture content, specific surface area and reconstitution time. The proposed models were validated with additional experiments, in which the responses observed were mainly in close agreement with the predicted ones. Additionally, the established models demonstrate the reliability of the evaluation procedure in predicting the selected responses.


2010 ◽  
Vol 26 (04) ◽  
pp. 1171-1176 ◽  
Author(s):  
LIU Xiang-Zhi ◽  
◽  
◽  
PIAO Ling-Yu ◽  
MAO Li-Juan ◽  
...  

2021 ◽  
Vol 250 ◽  
pp. 06010
Author(s):  
Lulu Niu ◽  
Jing Xie ◽  
Guangyong Li ◽  
Xuetong Zhang ◽  
Pengwan Chen

Graphene aerogel (GA) samples, prepared by the Sol-Gel method, were tested under quasi-static and dynamical compression, and characterized via surface area analyzer and scanning electron microscopy. The results show that the drying method has a significant influence on the sample’s microstructure as well as its mechanical compression properties. The supercritical CO2 dried sample has a notable higher specific surface area, and higher compression strength; although the freeze dried sample is much lighter than the supercritical CO2 dried sample, it exhibits a nonlinear superelastic behavior and large compressibility with a reversible strain up to 94%; under the dynamic compression test, the supercritical CO2 dried sample presents a negative Poisson’s ratio behavior whereas the flower-like failure pattern was observed for the freeze dried sample. GA, therefore, is a promising candidate for energy absorption purposes because of its very low density, high specific surface area and porous microstructure.


Gels ◽  
2019 ◽  
Vol 5 (1) ◽  
pp. 12 ◽  
Author(s):  
Victor Baudron ◽  
Pavel Gurikov ◽  
Irina Smirnova ◽  
Steve Whitehouse

The production of porous materials based on starch has been explored with supercritical drying—yielding aerogel—and freeze-drying. The two drying procedures were applied on the same gelling solution of amylomaize starch pasted at 140 °C and for two concentrations (5 and 10 wt.%). After gelation and retrogradation, water from the samples to be supercritically dried was exchanged to ethanol. The resulting starch aerogel presented high specific surface area (197 m2/g). Freeze-drying was assessed by investigating the effect of the gelation, retrogradation, freezing temperature, and sublimation pressure. The resulting starch materials were macroporous, with limited specific surface area and limited mechanical integrity. Cohesive open cell foam with pore size of ~20 µm was produced by quenching the hot starch melt in liquid nitrogen. The highest specific surface area obtained with freeze-drying was 7.7 m2/g for the hot starch melt frozen at −20 °C.


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