- Thermal hazard evaluation of cyclohexanone peroxide synthesis
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Cyclohexanone peroxide, a crucial organic peroxide used as a curing agent or an initiator in free radical polymerization, is produced through a reaction of cyclohexanone with hydrogen peroxide in the presence of nitric acid as the catalyst. For this study, we used reaction calorimeter, differential scanning calorimetry, and accelerating rate calorimeter to evaluate the thermal hazard characteristics of cyclohexanone peroxide synthesis and the thermal stability of cyclohexanone peroxide. The overall kinetic parameters of the peroxide reaction, which were calculated based on the Levenberg–Marquardt algorithm, were validated using experimental data. By combining the maximum temperature of the synthesis reaction that was corrected by the yield and temperature, at which time to the maximum rate under adiabatic decomposition conditions was equal to 24?h, criticality classes were depicted to assess the cooling failure scenario of the peroxide reaction. This study enhances our understanding of the peroxide reaction and presents safer operating conditions and design protection measures for a safer and greener chemical industry.
- Zang, Na,Qian, Xin-Ming,Liu, Zhen-Yi,Shu, Chi-Min
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- Over oxydone synthetic method (by machine translation)
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The invention belongs to the technical field of chemical synthesis, in particular relates to an over-oxydone synthetic method. Added to the organic solvent in the organic compounds, hydrogen peroxide and polyvinyl alcohol compound amino acid catalyst to stir dehydration reaction synthesis over oxydone; the polyvinyl alcohol composite amino acid catalyst by spherical polyvinyl alcohol precursor with the composite amino acid polymerization. The invention of peroxides in the production process, avoiding the use with the corrosive effect of chemical raw materials, optimization of the peroxide synthesis process, reduces the industrial production process of sodium chloride, sodium sulfate waste discharge. (by machine translation)
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Paragraph 0057-0058; 0059-0060; 0061-0062; 0069-0070
(2019/03/08)
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- Method for preparing ketone peroxide by ferrite compound as catalyst
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The invention discloses a method for preparing ketone peroxide by a ferrite compound as a catalyst. The method comprises that ketone and hydrogen peroxide undergo a reaction in the presence of a ferric oxide as a catalyst and the hydrogen peroxide is finally added when the temperature is raised to the reaction temperature. The ferric oxide replaces a titanium-silicon molecular sieve catalyst so that the cost of the catalyst is significantly reduced and the catalyst is easy to recover. The reaction conditions are low, the reaction conversion rate and selectivity are high under mild reaction conditions, the application range is wide, and the method can be used for production of a variety of ketones and its ketone peroxides and has very good application prospects.
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Paragraph 0021-0029
(2019/01/21)
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- Cyclohexanone peroxide preparation method
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The invention discloses a cyclohexanone peroxide preparation method. A titanium-silicon molecular sieve is taken as a catalyst, cyclohexanone and hydrogen peroxide undergo a reaction in a mild condition, and organic solvents, such as t-butyl alcohol and cyclohexane, are added. The reaction is completed in one step, the reaction system is quite simple, and the cyclohexanone conversion rate and cyclohexanone peroxide selectivity are high. The method is mild in reaction conditions, easy to control, simple in subsequent processing and friendly to the environment. Titanium-silicon molecular sieve is adopted as a catalyst and is easy to recycle and reused, and no side product is produced in the reaction.
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Paragraph 0016-0033
(2018/01/04)
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- Multi-sulfonic-acid-group acidic functionalized ionic liquid and preparation method thereof
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The invention provides multi-sulfonic-acid-group acidic functionalized ionic liquid, a preparation method thereof and a method of utilizing the ionic liquid to prepare organic peroxide.Each cation of the ionic liquid has two or three alkyl sulfonic acid side chains with 3 or 3 carbon atoms, a matched anion is hydrogen sulfate radical, and the ionic liquid is of an open straight chain structure.The preparation method of the organic peroxide includes: sequentially adding the ionic liquid and hydrogen peroxide into a reaction kettle, fully stirring at room temperature to homogeneous phase, adding cyclohexanone or methyl ethyl ketone, and finishing after reaction at room temperature for 3-8 h; separating a product out of a reaction system obtained through suction filtering or phase separation, sequentially performing water washing or saline washing to obtain water-phase liquid and a crude product, and drying the crude product under vacuum condition to obtain the organic peroxide.The preparation method has the advantages of mild reaction condition, high yield, high product purity and easiness in product separation.
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Paragraph 0067
(2017/01/02)
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- METHOD FOR PRODUCING ESTER OR LACTONE
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Disclosed is a method for producing an ester or lactone in which a secondary alcohol represented by following Formula (1) (wherein Ra and Rb each represent an organic group, or Ra and Rb may be combined to form a ring together with the adjacent carbon atom) is oxidized by molecular oxygen in the presence of a nitrogen-containing cyclic compound containing a structure represented by following Formula (I) [wherein X represents an oxygen atom or an -OR group (wherein R represents a hydrogen atom or hydroxyl-protecting group)] as a constituent of its ring, and at least one of a fluorine-containing alcohol and a fluorinated sulfonic acid, and thereby yields a compound represented by following Formula (2):
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Page/Page column 26
(2009/12/07)
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- PREPARATION OF TERMINAL ALKENIC ESTERS BY AN OXIDATIVE RADICAL REACTION
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A general method is described for the conversion of (mono)alkenic esters with the double bond at the nth C atom to terminal alkenic esters of (n-1) C atoms in length, with the double bond at n-2.Ozonolysis, either in methanol or in light petroleum, is followed by reaction with a mixture of ferrous and cupric salts.Methyl 10-undecenoate, methyl oleate (methyl (Z)-9-octadecenoate) and methyl erucate (methyl (Z)-13-docosenoate) were converted to methyl 8-nonenoate, methyl 7-ocotenoate and methyl 11-dodecenoate respectively.An improved preparation of 5-hexenoic acid is also described.
- Cardinale, G.,Laan, J. A. M.,Ward, J. P.
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p. 2899 - 2902
(2007/10/02)
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- Role of Hydroperoxides in the Ozonized Oxidation of Cycloalkanes
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Rate constants have been determined for the action of ozone on cyclohexyl and 1-methylcyclohexyl hydroperoxides, which are formed by the oxidation of of cyclohexane and methylcyclohexane respectively.The reactivity of peroxy-compounds towards ozone diminishes in the sequence-cyclohexylhydroperoxide (I) > peroxydicyclohexane-1,1'-diol (IV) > 1,1'-hydroperoxycyclohexylperoxycyclohexanol (III) > peroxy-1,1'-dicyclohexane dihydroperoxide (V) > 1-methylcyclohexylhydroperoxide (II).
- Vikhorev, A. A.,Syroezhko, A. M.,Proskuryakov, V. A.,Korotkova, N. P.
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p. 251 - 253
(2007/10/02)
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- Ketone-derived Peroxides. Part I. Synthetic Methods.
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Study of the reactivity of peroxides derivable from ketones by reaction with hydrogen peroxide has required reexamination of preparative methods.Conditions for obtaining five known peroxides from cyclohexanone and the new 1-(1-hydroxycyclohexyldioxy)-1-(1-hydroperoxycyclohexyldioxy)cyclohexane (10) are carefully defined.An improved general method for obtaining cyclic diperoxides (3,3,6,6-tetrasubstituted 1,2,4,5-tetraoxans) (6) has been developed and used to obtain new diperoxides from dibenzyl ketone, di-(4-methylbenzyl) ketone and 2,2-dimethylcyclohexanone whereas indan-2-one and 5,7-dihydro-6H-dibenzocyclohepten-6-one yield the corresponding triperoxides (1,2,4,5,7,8-hexoxonans) (7) and 1,5-diphenylpentan-3-one yields bis-(1-hydroperoxy-1-phenethyl-3-phenylpropyl) peroxide (5k).Ozonolysis of appropriate alkenes has been used to obtain new cyclic diperoxides formally related to 4'-methylacetophenone, propiophenone and deoxybenzoin.
- McCullough, Kevin J.,Morgan, Alistair R.,Nonhebel, Derek C.,Pauson, Peter L.,White, Graham J.
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p. 601 - 628
(2007/10/02)
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