The Process of Phenol Hydroxylation in the Water Solution and over the Ti-MWW Catalyst

Author(s):  
Agnieszka Wróblewska

Abstract This work presents the studies on the optimization of the process of phenol hydroxylation over the Ti-MWW catalyst. The medium of the reaction was only water introduced into the rector with the 30 wt% hydrogen peroxide (oxidizing agent) and formed during the reaction from the hydrogen peroxide. For the mathematical optimization the rotatable-uniform design was used. The main investigated technological parameters were: the temperature, the molar ratio of phenol/hydrogen peroxide, the catalyst content and the reaction time. The course of the main functions describing the process were presented in the form of layer drawings. The analysis of the layer drawings allowed to establish the most beneficial parameters for this process. Studies have shown that in water solution it is best to conduct phenol hydroxylation process at: the temperature of 93-100oC, phenol/hydrogen peroxide molar ratio 0.9-1, catalyst concentration 3-3.5 wt% and during the reaction time of 55-60 minutes. Under these conditions, it is possible to achieve phenol conversion of 85 mol%, selectivity of transformation to organic compounds in relation to phenol consumed 50 mol% and the yield of hydroquinone about 19 mol%. The phenol hydroxylation method, presented in this article, is a preferred alternative to conventional solutions, as it is more environmentally and cost-effective, taking into account consumption of raw materials and energy.

2012 ◽  
Vol 15 (2) ◽  
Author(s):  
Agnieszka Wróblewska

AbstractsAs a result of phenol hydroxylation, two useful products can be received: hydroquinone and pyrocatechol. In this work the hydroxylation of phenol with hydrogen peroxide over the Ti-MWW catalyst has been studied. Optimization studies were performed by application of a statistical experimental design method utilizing a rotatable-uniform design. The influence of five parameters on the course of this process was examined: temperature (120-150°C), molar ratio of phenol/hydrogen peroxide (0.5-1.5), acetonitrile - solvent content (20- 50 wt%), catalyst - Ti-MWW content (8-18 wt%) and reaction time (60-120 min). The process description was based on four response functions: the conversion of phenol to organic compounds, the yield of pyrocatechol, the yield of hydroquinone and the conversion of phenol to tars. The most favourable parameters for the process of phenol hydroxylation were as follows: temperature 147-150°C, molar ratio of phenol/hydrogen peroxide 0.5-0.6, acetonitrile content 21-24 wt%, Ti-MWW content 10.3-10.6, reaction time 221-236 min. In summary, these the most favourable parameters allow one to obtain pyrocatechol with the yield of 18 mol%, hydroquinone with the yield of 20 mol%, at the conversion of phenol to organic compounds 38 mol% in relatively mild and safe conditions. These results also showed that Ti-MWWcatalyst can be a good substitute for TS-1 catalyst.


2015 ◽  
Vol 17 (4) ◽  
pp. 23-31 ◽  
Author(s):  
Agnieszka Wróblewska ◽  
Edyta Makuch ◽  
Małgorzata Dzięcioł ◽  
Roman Jędrzejewski ◽  
Paweł Kochmański ◽  
...  

Abstract This work presents the studies on the optimization the process of allyl alcohol epoxidation over the Ti-SBA-15 catalyst. The optimization was carried out in an aqueous medium, wherein water was introduced into the reaction medium with an oxidizing agent (30 wt% aqueous solution of hydrogen peroxide) and it was formed in the reaction medium during the processes. The main investigated technological parameters were: the temperature, the molar ratio of allyl alcohol/hydrogen peroxide, the catalyst content and the reaction time. The main functions the process were: the selectivity of transformation to glycidol in relation to allyl alcohol consumed, the selectivity of transformation to diglycidyl ether in relation to allyl alcohol consumed, the conversion of allyl alcohol and the selectivity of transformation to organic compounds in relation to hydrogen peroxide consumed. The analysis of the layer drawings showed that in water solution it is best to conduct allyl alcohol epoxidation in direction of glycidol (selectivity of glycidol 54 mol%) at: the temperature of 10–17°C, the molar ratio of reactants 0.5–1.9, the catalyst content 2.9–4.0 wt%, the reaction time 2.7–3.0 h and in direction of diglycidyl ether (selectivity of diglycidyl ether 16 mol%) at: the temperature of 18–33°C, the molar ratio of reactants 0.9–1.65, the catalyst content 2.0–3.4 wt%, the reaction time 1.7–2.6 h. The presented method allows to obtain two very valuable intermediates for the organic industry.


2011 ◽  
Vol 14 (2) ◽  
Author(s):  
Agnieszka Wróblewska ◽  
Grzegorz Wójtowicz ◽  
Edyta Makuch

AbstractThis work presents the results of phenol hydroxylation with hydrogen peroxide over the Ti-MWW catalyst. The studies were carried out under autogenic pressure and in the presence of acetonitrile as a solvent. The influence of the following technological parameters on the course of hydroxylation was examined: the temperature in the range of 100-150 °C, the molar ratio of phenol/H


2017 ◽  
Vol 19 (1) ◽  
pp. 11-16 ◽  
Author(s):  
Shuang Zhang ◽  
Long Zhang

Abstract In this paper, 2,5-furandicarboxylic acid (FDCA) was efficiently prepared by the direct oxidation of 5-hydroxymethylfurfural (5-HMF) using hydrogen peroxide (H2O2) in alkaline conditions without any catalysts. The effects of reaction parameters on the process were systematically investigated and the optimal parameters were obtained as follows: molar ratio of 5-HMF:KOH:H2O2 was 1:4:8, reaction temperature and reaction time were determined as 70°C and 15 minutes, respectively. Under these conditions, the yield of FDCA was 55.6% and the purity of FDCA could reach 99%. Moreover, we have speculated the detailed oxidation mechanism of 5-HMF assisted by hydrogen peroxide in alkaline condition to synthesize FDCA.


2011 ◽  
Vol 298 ◽  
pp. 163-168 ◽  
Author(s):  
Yuan Yuan Lei ◽  
Guo Zheng ◽  
Yu Sun ◽  
Yong Zhou

In this paper, with fatty alcohol polyoxyethylene (AEO9), succinic anhydride (SA) and sodium hydroxide as raw materials, a new type of fatty alcohol polyoxyethylene carboxylate surfactants (SAE9C-Na) was obtained by esterification and neutralizing effect. The influencing factors were researched and its surface properties were studied. The optimum condition of synthesis was determined: molar ratio of alcohol to acid was 1:1.1, reaction temperature was 85°C, reaction time was 60 min, under this condition, the yield could reach up to 95.8%. The results received from this experiment showed that SAE9C-Na had excellent surface activity and foaming and foam stability, whose emulsification and solubility enhancement were improved greatly.


2015 ◽  
Vol 659 ◽  
pp. 216-220 ◽  
Author(s):  
Achanai Buasri ◽  
Thaweethong Inkaew ◽  
Laorrut Kodephun ◽  
Wipada Yenying ◽  
Vorrada Loryuenyong

The use of waste materials for producing biodiesel via transesterification has been of recent interest. In this study, the pork bone was used as the raw materials for natural hydroxyapatite (NHAp) catalyst. The calcination of animal bone was conducted at 900 °C for 2 h. The raw material and the resulting heterogeneous catalyst were characterized using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and the Brunauer-Emmett-Teller (BET) method. The effects of reaction time, microwave power, methanol/oil molar ratio, catalyst loading and reusability of catalyst were systematically investigated. The optimum conditions, which yielded a conversion of oil of nearly 94%, were reaction time 5 min and microwave power 800 W. The results indicated that the NHAp catalysts derived from pork bone showed good reusability and had high potential to be used as biodiesel production catalysts under microwave-assisted transesterification of Jatropha Curcas oil with methanol.


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.


2016 ◽  
Vol 18 (4) ◽  
pp. 9-14 ◽  
Author(s):  
Marika Walasek ◽  
Agnieszka Wróblewska

Abstract This work presents the studies on the epoxidation of allyl-glycidyl ether (AGE) over the Ti-SBA-15 catalyst. In these studies an aqueous hydrogen peroxide was used as an oxidizing agent and as a solvent methanol was applied. The studies on the influence the following parameters: temperature (20–80°C), molar ratio of AGE/H2O2 (1:1.5–5:1), methanol concentration (10–90 wt%), catalyst content (1–9 wt%) and reaction time (15–240 min.) were carried out and the most favourable values of these parameters were chosen (temperature 80°C, molar ratio of AGE/H2O2 = 5:1, methanol concentration 30 wt%, catalyst content 3 wt% and the reaction time 240 min.). At these conditions the functions describing the process reached the following values: the selectivity of diglycidyl ether (DGE) 9.2 mol%, the conversion of AGE 13.9 mol% and the efficiency of H2O2 conversion 89.9 mol%.


2011 ◽  
Vol 66-68 ◽  
pp. 65-69
Author(s):  
Long Feng Li ◽  
Yuan Gao ◽  
Mao Lin Zhang

Ca-Mg-Al hydrotalcite-like compounds (CaMgAl-HTLcs) were synthesized by a hydrothermal method, and characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and differential thermal analysis (DTA) techniques. The effects of the medium pH value, the molar ratio of the raw materials, the reaction temperature and the reaction time on the structure of CaMgAl-HTLcs were studied. The results showed that increasing treatment temperature and reaction time could improve the crystallinity and monodispersity of hydrotalcite-like compound particles. And well-defined CaMgAl-HTLcs could be prepared at a pH value of 10~11 with n(Zn+Mg+Ca):n(Al) =2. The products synthesized were applied to PVC to improve the thermal stability of PVC.


2019 ◽  
Vol 6 (3) ◽  
pp. 185-190
Author(s):  
Ali Abdul Rahman-Al Ezzi ◽  
Salam H. Alhamdiny

Background: Several important designs have been applied to remove toxic and hazardous organic substances like phenol and phenol compounds from wastewater, but there is a need to seek an alternative design to effectively remove organic pollutants from water to less hazardous compounds and a costeffective system. Methods: A modified internal loop airlift reactor was designed to remove the organic pollutants in synthetic wastewater using an efficient and cost-effective treatment technique by means of a synergistic effect of combination oxidation, stripping, and adsorption. The influence of the current style was experimentally examined in the treatment of synthetic phenol contaminated wastewater. The practical device was tested under different airflow rates range (2-15 L/min) through gross difference retention period (5-60 minutes) at a various molar ratio of phenol to hydrogen peroxide ranging from 1:10 to 1:20. Results: It was revealed that the preferred molar ratio of phenol to hydrogen peroxide equals to 1:20. Moreover, the airflow rate is 15 L/min with longer retention period of 60 minutes, indicating the maximum removal efficiency (89%) of phenol from the synthetic wastewater. Conclusion: Successful removal of phenol from water by the removal efficiency of 89% boosts the success of the executed design as well as the scenario of conducting the synergistic processes (stripping, oxidation and adsorption) in one device and also increases the chances of solving environmental problems via treating wastewater before recycling and releasing it into natural water sources.


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