A new method for the preparation of peroxymonophosphoric acid

2003 ◽  
Vol 81 (2) ◽  
pp. 156-160 ◽  
Author(s):  
Tian Zhu ◽  
Hou-min Chang ◽  
John F Kadla

A new method for the preparation of peroxymonophosphoric acid (H3PO5) has been developed. It utilizes a biphasic solution to moderate the vigorous reaction between phosphorous pentoxide (P2O5) and hydrogen peroxide (H2O2). P2O5 is suspended in carbon tetrachloride (CCl4), and concentrated H2O2 is slowly added while being vigorously stirred at low temperature. Careful control of the reaction temperature through the slow addition of H2O2 is critical. Using typical preparation conditions (P2O5:H2O2 = 0.5:1, H2O2 70 wt %, 2°C, 120–180 min), ~70% of the H2O2 is effectively converted to H3PO5. Increasing the concentration of H2O2, as well as the mole ratio of P2O5:H2O2, leads to an even higher % conversion of H2O2 to H3PO5. The addition of glacial acetic acid to the P2O5:H2O2 suspension at the end of the 120–180 min reaction (P2O5:H2O2:CH3COOH = 0.5:1:0.3) leads to the formation of peracetic acid in addition to H3PO5, and to an overall increase in the conversion ratio of total peroxy acids based on H2O2 (>95%).Key words: peroxymonophosphoric acid, synthesis, stability, conversion ratio.

1972 ◽  
Vol 55 (1) ◽  
pp. 57-59
Author(s):  
Joel J Thrasher

Abstract A collaborative study has been completed on a new method for light filth in ground coffee. The sample is defatted with chloroform, dried, and boiled in water; isopropanol is added and the sample is boiled again. Light filth is trapped off with mineral oil from a hot solution. The method yields better recoveries of insect fragments and rodent hairs than the official method. Other advantages are less analytical time, cleaner filter papers, and elimination of the use of carbon tetrachloride. It is recommended that the method be adopted as official first action to replace 40.007(b) for the isolation of light filth from ground coffee and that the hydrogen peroxide bleaching technique described earlier be adopted as a procedure to replace the sodium hypochlorite technique described in 40.006.


2013 ◽  
Vol 25 (2) ◽  
pp. 124-131
Author(s):  
Mohammad Shahid Ullah ◽  
M Giasuddin Ahmed ◽  
UKR Romman ◽  
Kawsari Akhter ◽  
S Mosaddeq Ahmed ◽  
...  

Some 5, 7-diaryl-1,5-dihydro (or 1, 2, 3, 5-tetrahydro)- pyrano[2, 3-d] pyrimidin-2, 4- diones (or 2-thioxo-4-ones) (3a-g) has been synthesized in one-step by the cyclocondensation of barbituric acid or thiobarbituric acid (1) with arylideneacetophenones (2a-d), in glacial acetic acid in the presence of phosphorous pentoxide. The structures of the compounds 3a-g were determined by their UV, IR, 1H NMR, 13C NMR, mass spectral data and elemental analyses. Journal of Bangladesh Chemical Society, Vol. 25(2), 124-131, 2012 DOI: http://dx.doi.org/10.3329/jbcs.v25i2.15064


ACS Omega ◽  
2020 ◽  
Vol 5 (12) ◽  
pp. 6389-6394
Author(s):  
Yingjie Zhang ◽  
Guanqun Gong ◽  
Honglei Zheng ◽  
Xin Yuan ◽  
Liangwei Xu

1959 ◽  
Vol 37 (2) ◽  
pp. 366-369 ◽  
Author(s):  
Paul E. Gagnon ◽  
Brian T. Newbold

A series of dihalogenated and five tetrachloroazobenzenes were oxidized to the corresponding azoxy compounds by means of 30% hydrogen peroxide in glacial acetic acid, the reaction being carried out at about 60–70 °C, for 24 hoursAs expected, the yields, in general, obtained from azobenzenes containing substituents in the 2,2′-positions were lower than those from compounds having substituents in the 3,3′- and 4,4′-positions, which gave very good results.


2008 ◽  
Vol 5 (s1) ◽  
pp. 1063-1068 ◽  
Author(s):  
Yogesh Dixit ◽  
Rahul Dixit ◽  
Naveen Gautam ◽  
D. C. Gautam

The present communication deals with the synthesis of a series of fluorinated 10H-phenothiazines. 10H-phenothiazines is prepared by Smiles rearrangement of substituted 2-foramido-2´-nitrodiphenylsulfide. Substituted 2-foramido-2´-nitrodiphenylsulfide were obtained by the reaction of 2-amino-3-fluorobenzenethiol witho-halonitrobenzenes followed by formylation and 1-nitro/1-halo-10H-phenothiazines have been prepared by the reaction of substituted 2-aminobenzenethiols with reactiveo-halonitrobenzene containing a nitro group or halogen atom ato-position to the reactive halogen atom directly yielded 1-nitro/1-halo-10H-phenothiazines in situ. 10H-phenothiazine sulfone derivatives have been synthesized by the oxidation of 10H-phenothiazines by 30% hydrogen peroxide in glacial acetic acid. The structure of the synthesized compounds has been characterized by spectroscopic data and elemental analysis. Antimicrobial studies of the synthesized compounds have also been included.


1970 ◽  
Vol 41 (3) ◽  
pp. 119-128 ◽  
Author(s):  
MG Ahmed ◽  
UKR Romman ◽  
SM Ahmed ◽  
Khondaker Akhter ◽  
ME Halim ◽  
...  

5,7-Diphenyl-1,2,3,4-tetrahydro-2,4-dioxo-5H-pyrano[2,3-d]pyrimidine (4a) has been synthesized in single-step by the condensation of barbituric acid (1) with benzylideneacetophenone (2a) in glacial acetic acid in the presence of phosphorous pentoxide. Reaction of barbituric acid (1) with arylideneacetophenones (2b-d) which gave the corresponding adducts of 5-(1,3-diaryl-1-oxopropyl) pyrimidine (1H, 3H, 5H)-2,4,6-triones (3a-c) previously in 50 % aqueous ethanol which on further reflux in gl. acetic acid in the presence of phosphorous pentoxide also gave the corresponding pyranopyrimidines 5,7-diaryl-1,2,3,4-tetrahydro-2,4-dioxo-5H-pyrano [2,3- d]pyrimidines (4b-d). The structures of the compounds 4a-d were characterized by their UV, IR, 1H NMR and 13C NMR spectral data. Bangladesh J. Sci. Ind. Res. 41(3-4), 119-128, 2006


Author(s):  
Ferra Naidir ◽  
Robiah Yunus ◽  
Irmawati Ramli ◽  
Tinia I. Mohd. Ghazi

To improve the oxidative stability of the palm oil-based biolubricant, the fatty acid double bonds in palm oil-based trimethylolpropane ester (TMP ester) was converted into an oxirane ring via an in-situ epoxidation method. The epoxidized TMP ester was produced from a reaction between TMP ester and peracetic acid which was prepared in-situ by reacting glacial acetic acid with hydrogen peroxide in the presence of concentrated sulphuric acid. The response surface methodology was applied using a central composite design technique to optimize the conditions of the epoxidation reaction to produce the epoxidized TMP ester. The effects of four independent variables namely concentration of acetic acid (0-2 mol), concentration of hydrogen peroxide (1.5-9.5 mol), temperature of reaction (30-110°C) and reaction time (0.5-26.5 h) on the three dependent variables; percentage of oxirane oxygen, iodine value, and hydroxyl value were studied. A second-order polynomial multiple regression model was employed to predict the three dependent variables under optimum conditions of 0.59 mol of glacial acetic acid, 7.5 mol of hydrogen peroxide concentration, at temperature of 50°C and reaction times of 7 h. The optimum values of percentage of oxirane oxygen, iodine value, and hydroxyl value were 4.01%, 1.94%, and 0.43% respectively. The analysis of variance yielded a high coefficient of determination value of 0.9395-0.9880, hence indicating the fitness of the second-order regression model to the experimental data.


2017 ◽  
Vol Volume-1 (Issue-6) ◽  
pp. 1271-1275
Author(s):  
Bach Trong Phuc ◽  
Vu Van Hai ◽  
Nguyen Thi Hien | Nguyen Thanh Liem ◽  

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