scholarly journals One-Step Synthesis of Hydroxysodalite Using Natural Bentonite at Moderate Temperatures

Minerals ◽  
2018 ◽  
Vol 8 (11) ◽  
pp. 521 ◽  
Author(s):  
Bo Liu ◽  
Hongjuan Sun ◽  
Tongjiang Peng ◽  
Qian He

Ca-bentonite was used as the feedstock material for the synthesis of hydroxysodalite due to its high Al, Si content, good chemical reactivity, and natural abundance. A one-step method is proposed here to fabricate hydroxysodalite in a water bath at moderate temperature. The effects of the Na/Si molar ratio, Si/Al molar ratio, reaction time, and reaction temperature on the synthesis of hydroxysodalite have been systematically investigated here. The crystallizing phases and morphology of the synthetic products were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results showed that the Na/Si molar ratio and reaction temperature both played important roles in controlling the degree of crystallinity of the synthetic hydroxysodalite. The Si/Al molar ratio and reaction time both affect the purity of the synthetic hydroxysodalite. Optimum conditions for synthesizing hydroxysodalite using a one-step water-bath method at moderate temperature are as follows: a Na/Si molar ratio of 12, a Si/Al molar ratio of 1.0, a reaction temperature of 90 °C, and a reaction time of 12 h.

2019 ◽  
Vol 21 (3) ◽  
pp. 35-39
Author(s):  
Chuanbo Dai ◽  
Hongyu Zhang ◽  
Ruiduan Li ◽  
Haifeng Zou

Abstract Herein, a simple and effective method for the preparation of thiourea using a nucleophilic substitution reaction is reported. Urea and Lawesson’s reagent were used as the raw materials to prepare thiourea via a one-step method involving the sulfuration reaction, and the reaction mechanism was analyzed. The effect of the reaction time, reaction temperature, and mass ratio of the raw materials on the yield of thiourea were investigated.The most beneficial conditions used for the reaction were determined to be: Reaction time = 3.5 h, reaction temperature = 75°C, and mass ratio of urea to Lawesson’s reagent = 2:1. Under these optimal conditions, the average yield of thiourea over five replicate experiments was 62.37%. Characterization using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) and thermogravimetric analysis (TGA) showed that the as-synthesized substance was thiourea. Our synthetic method has the advantages of high yield, mild reaction conditions and simplicity.


2017 ◽  
Vol 17 (2) ◽  
pp. 309 ◽  
Author(s):  
Nurhayati Nurhayati ◽  
Sofia Anita ◽  
Tengku Ariful Amri ◽  
Amilia Linggawati

In this study biodiesel was produced from crude palm oil through two-step processes, namely esterification reactions using homogeneous H2SO4 catalyst and transesterification using the heterogeneous base CaO catalyst derived from Anadara granosa shell. Several parameters affecting to the yields of biodiesel were investigated including the amount of the catalysts, the molar ratios of oil to methanol, reaction times and reaction temperatures. The CaO catalyst was prepared by calcining the A. granosa shells at the temperatures of 800 and 900 °C for 10 h. The as-synthesized biodiesel was analyzed using GC and its characteristics were determined and the results were compared to Standard National for Biodiesel (SNI 04-7183-2006). The optimum condition for the esterification process (step 1) was as follows: reaction temperature of 65 °C, reaction time of 3 h and mol ratio of oil to methanol 1:24. For the transesterification (step 2) the optimum conditions were attained using the catalyst weight 3%, reaction temperature of 60 °C, reaction time of 3 h, mole ratio of oil/methanol 1:6 and the catalyst calcination time of 10 h with the conversion of 87.17%. This biodiesel yield by the two-step processes was higher (2.7%) than that using only one-step process (transesterification).


2019 ◽  
Vol 19 (4) ◽  
pp. 849
Author(s):  
Nurul Atikah Amin Yusof ◽  
Nursyamsyila Mat Hadzir ◽  
Siti Efliza Ashari ◽  
Nor Suhaila Mohamad Hanapi ◽  
Rossuriati Dol Hamid

Optimization of the lipase catalyzed enzymatic synthesis of betulinic acid amide in the presence of immobilized lipase, Novozym 435 from Candida antartica as a biocatalyst was studied. Response surface methodology (RSM) and 5-level-4-factor central-composite rotatable design (CCRD) were employed to evaluate the effects of the synthesis parameters, such as reaction time (20–36 h), reaction temperature (37–45 °C), substrate molar ratio of betulinic acid to butylamine (1:1–1:3), and enzyme amounts (80–120 mg) on the percentage yield of betulinic acid amide by direct amidation reaction. The optimum conditions for synthesis were: reaction time of 28 h 33 min, reaction temperature of 42.92 °C, substrate molar ratio of 1:2.21, and enzyme amount of 97.77 mg. The percentage yield of actual experimental values obtained 65.09% which compared well with the maximum predicted value of 67.23%. The obtained amide was characterized by GC, GCMS and 13C NMR. Betulinic acid amide (BAA) showed a better cytotoxicity compared to betulinic acid as the concentration inhibited 50% of the cell growth (IC50) against MDA-MB-231 cell line (IC50 < 30 µg/mL).


Holzforschung ◽  
2007 ◽  
Vol 61 (5) ◽  
pp. 499-503 ◽  
Author(s):  
Shifa Wang

Abstract A light-colored rosin glycerol ester was synthesized from gum rosin and glycerol in the presence of a highly effective decolorizing agent. The effects of the type and dosage of the decolorizing agent and the reaction temperature and time on the yield, softening point, color, and acid number of the rosin glycerol ester were investigated. Experimental results showed that 4,4′-thio-bis(6-tert-butyl-3-methyl phenol) was the best decolorizing agent. It promoted esterification at an optimal dosage of 0.5% (based on the weight percentage of starting material rosin). Suitable conditions for esterification of rosin and glycerol were: reaction temperature, 260–270°C; reaction time, 6–8 h; and rosin/glycerol molar ratio, 2.5:1 (mol mol-1). The characteristics of the rosin glycerol ester obtained under these conditions were as follows: softening point, 90–94°C (ball and ring method); color, 1–2 (Gardner value); acid number, 7–8; and yield, >88% (based on the total weight of rosin and glycerol). The selected additive has a multifunctional effect involving bleaching, disproportionation, and catalysis.


2019 ◽  
Vol 2019 ◽  
pp. 1-12 ◽  
Author(s):  
Xiaoling Yao ◽  
Chungui Du ◽  
Yating Hua ◽  
Jingjing Zhang ◽  
Rui Peng ◽  
...  

In recent years, bamboo has been widely used for building materials and household goods. However, bamboo is flammable, so a flame-retardant treatment for bamboo is urgently needed. In this work, nano MgAl-layered double hydroxide (MgAl-LDH) coated on bamboo, which was called MgAl-LB, was synthesized by an in situ one-step method. To determine the optimal in situ time, the effects of different reaction times on LDH growth on the bamboo surface and the flame retardancy of the MgAl-LBs were investigated. The SEM observations show that LDH growth on the surface of bamboo was basically saturated when the in situ reaction time was 24 h. Abrasion experiments show that MgAl-LDH coating has good abrasion resistance. The fire performance of the MgAl-LBs was evaluated by cone calorimeter tests, which indicated that the THR and TSP of the MgAl-LBs were significantly lower than those of untreated bamboo. Taking into account the energy consumption problem, determining the reaction time of 24 h is the optimal reaction time. Compared with untreated bamboo, the THR and TSP of MgAl-LB prepared at 24 h decreased by 33.3% and 88.9%, respectively.


Synlett ◽  
2020 ◽  
Vol 31 (12) ◽  
pp. 1205-1210 ◽  
Author(s):  
Guo-Sheng Huang ◽  
Xin-Feng Cui ◽  
Fang-Peng Hu ◽  
Xiao-Qiang Zhou ◽  
Zhen-Zhen Zhan

A ruthenium-catalyzed [5+1] annulation of 1-(2-aminophenyl)pyrroles with α-carbonyl sulfoxonium ylides is reported. This reaction provides a one-step method for synthesizing pyrrolo[1,2-a]quinoxaline derivatives under ambient conditions. The system proceeds with a short reaction time and a high functional-group tolerance. Notably, this divergent protocol tolerates β-keto sulfoxonium ylides and can be applied to α-ester sulfoxonium ylides. A preliminary study was made of the mechanism of the reaction, and a reaction pathway is proposed.


2019 ◽  
Vol 953 ◽  
pp. 185-190
Author(s):  
Yong Li Peng ◽  
Ni An Zhuo ◽  
Can Zhang

A new phosphorus-containing flame-retardant curing agent PPDTA was synthesized from phenylphosphonic dichloride (PPD) and 3-amino-1,2,4-triazole (TA) in tetrahydrofuran solvent to improve the flame retardancy of epoxy resin. The structure of the compound was analyzed and confirmed by infrared spectroscopy. The effects of reaction time, reaction temperature and ratio of reactants on yield were studied by using three-factor three-level orthogonal experiment. The results show that the yield of PPDTA can reach 86.4%, when the reaction time is 10h, reaction temperature is 70 °Cand the molar ratio of TA to PPD is 2.2:1.


2013 ◽  
Vol 781-784 ◽  
pp. 526-530 ◽  
Author(s):  
Shao Ying Li ◽  
Chun Mei Niu ◽  
Hua Yu Zhong

Series of cationic cassia tora gum (CCTG) were synthesized using 3-chloro-2-hydroxypropyl trimethyl ammonium chloride (CHPTAC) as cationic etherifying agent, isopropanol-water solution as dispersing agent, in presence of sodium hydroxide under different reaction conditions. The optimum ratio for preparing the cationic cassia tora gum are that CHPTAC-CTG molar ratio is 0.6:1; NaOH-CHPTAC molar ratio is 1.3:1.The optimum conditions are that reaction temperature is 55°Cand reaction time is 3.5 h. The cold water solubility was improved apparently. The solution transmittance has corresponding relationship with the nitrogen content (N%) in the certain range, and the maximum transmittance is up to 87.2%. N% increased with the increase of reaction time and stable N% can be obtained in shorter reaction time at higher reaction temperature. The products were characterized by 13C-NMR. The heat resistance of CTG and CCTG were analyzed.


2012 ◽  
Vol 9 (2) ◽  
pp. 545-552 ◽  
Author(s):  
Yan-Hua Cai ◽  
Shun-Jiang Li

N-(benzoyl) stearic acid hydrazide was synthesized from benzoyl hydrazine and stearyl chloride which was deprived from stearic acid via acylation. The structure of the compound had been characterized by FT-IR,1H NMR, at the same time, the structure of N-(benzoyl) stearic acid hydrazide was optimized by the semiempirical method PM3. The influence of the reaction ratio, reaction time and reaction temperature to the yield ofN-(benzoyl) stearic acid hydrazide was investigated by orthogonal experiment, and the optimized reaction condition was molar ratio of benzoyl hydrazine: stearyl chloride 1:1, reaction time 6 h, reaction temperature 70°C, and the yield was 92.9%. The TGA thermal analysis of N-(benzoyl) stearic acid hydrazide showed that thermal stability ofN-(benzoyl) stearic acid hydrazide was affected by heating rate, and theN-(benzoyl) stearic acid hydrazide enhanced the tensile strength, modulus and elongation at break of Poly(L-lactic acid)(PLLA).


2013 ◽  
Vol 634-638 ◽  
pp. 628-631
Author(s):  
Yun Hui Long ◽  
Jun Ming Guo ◽  
Du Shu Huang ◽  
Gui Yang Liu

The catalytic synthesis of ethyl acetate from ethanol and acetic acid using Ti2SnC in liquid phase under the atmospheric pressure was studied. The influences of some factors such as catalyst usage, initial reactant molar ratio, reaction temperature and reaction time on acetic acid conversion rate of this reaction system were investigated. The acetic acid conversion rate of 88.12% is achieved while the molar ratio of alcohol and acid is 1:3.6, the amount of catalyst is 0.2000 g, the reaction temperature is 80 °C and the reaction time is 30min. The catalyst Ti2SnC is the ideal catalyst for synthesis of ethyl acetate for good catalytic performance, non-corrosive to equipment, easily separated from product and used repeatedly.


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