- High-pressure preparation method of tetra[beta-(3,5-di-tert-butyl-4-hydroxy phenyl)propanoic acid]pentaerythritol ester
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The invention relates to a high-pressure preparation method of tetra[beta-(3,5-di-tert-butyl-4-hydroxy phenyl)propanoic acid]pentaerythritol ester. The technical scheme adopted by the method disclosed by the invention lies in that beta-(3,5-di-tert-butyl-4-hydroxy phenyl)methyl propionate, pentaerythritol, a catalyst and an organic solvent are enabled to be subjected to a reaction at the pressure of 3-4MPa and at the temperature of 130-140 DEG C for 7-9h so as to obtain the tetra[beta-(3,5-di-tert-butyl-4-hydroxy phenyl)propanoic acid]pentaerythritol ester. The high-pressure preparation method disclosed by the invention is simple, capable of utilizing waste and low in energy consumption, and the purity of the obtained tetra[beta-(3,5-di-tert-butyl-4-hydroxy phenyl)propanoic acid]pentaerythritol ester is high.
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Paragraph 0017; 0018; 0019
(2017/02/09)
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- Method for preparing hindered phenol antioxygen 1010
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The invention belongs to the technical field of fine chemistry, and in particular relates to a method for preparing a hindered phenol antioxygen 1010. According to the method provided by the invention, beta-(3,5-ditert-butyl-4-hydroxyphenyl)methyl propionate and pentaerythrotol are used as raw materials and are subjected to ester exchange reaction to obtain the hindered phenol antioxygen 1010; the ester exchange reaction is carried out in an alkaline ion liquid catalysis system. According to the method provided by the invention, alkali ion liquid is used as a catalyst and the catalytic activity is high; the content of a product reaches 97.5 percent or more, and the yield reaches 95 percent or more. The performance of the alkaline liquid catalyst in 1010 esterification reaction is better that that of catalysts including lithium acetate, sodium methoxide, potassium tert-butoxide, organic tin and the like. An ion liquid catalytic reaction system is used and is environmentally friendly; the catalyst can be cyclically utilized; a product is not easily colored, has high yield and does not contain heavy metal.
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Paragraph 0031; 0032; 0033; 0034; 0035; 0036; 0037-0050
(2017/08/29)
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- Transesterification of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoate with tetrakis(hydroxymethyl)methane. the properties of the reaction products
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The transesterification of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoate with tetrakis(hydroxymethyl)methane depends on the equilibrium constants of the reversible reactions; for the final step, the equilibrium constant is K 1. The molecular geometries and the enthalpies and entropies of the equilibrium reactions were calculated by the semiempirical PM6 quantum chemical method. The thermodynamic equilibrium constants of the reversible reactions were calculated by the Boltzmann equation from the Gibbs energies G f ○. For tris-[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoyloxymethyl](hydroxymethyl)methane, the dipole moment is μ = 0.97 D and the energy of the O-H homolysis is D OH = 347.3 kJ mol -1. For tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoyloxymethyl]methane, μ is 5.6 D and D OH is 321 kJ mol -1. The geometry of the structure affects the H-O homolysis energy and the chain termination coefficient under the conditions of inhibited cumene oxidation.
- Volod'Kin,Zaikov,Evteeva
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p. 1689 - 1693
(2013/11/19)
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- PREPARATION OF TETRAKIS [3-(E,5-DI-TERT-BUTYL-4-HYDROXY PHENYL) PROPIONYL OXYMETHYL] METHANE
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A transesterification process for the preparation of tetrakis [3-(3,5-di-tert-butyl-4hydroxy phenyl) propionyl oxymethyl] methane by the reaction of methyl-(3,5-di-tertbutyl-4-hydroxy phenyl) propionate ester with pentaerythritol wherein the reaction takes place in the presence of an ester exchange catalyst combination consisting of (a) at least one basic or neutral catalyst and (b) at least one metal compound capable of behaving as a Lewis acid and wherein the reaction is conducted through a first stage in which only basic or neutral catalyst is present in the reaction mixture followed by a second stage which commences with the addition of Lewis acid catalyst to the reaction mixture when the amount of di-substituted intermediate product contained within the reaction mixture is less than 20 area % analysed by HPLC. The preferred basic catalysts are lithium hydroxide and lithium hydroxide monohydrate. The preferred Lewis acid catalyst is zinc octanoate.
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Page/Page column 10
(2008/06/13)
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- PHENOLIC ANTIOXIDANTS IN CRYSTALLINE FORM
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The invention relates to a process for preparing solid particles of a phenolic antioxidant from the IRGANOX series in the form of crystals, particularly IRGANOX 1010 and 1098, the crystal particles obtainable by the process, the further processing of the crystal particles, an aqueous dispersion comprising the phenolic antioxidant, novel crystal modifications of pentaerythritol tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionate] (μ -form) and N,N'-hexane-1,6diyl-bis[3-(3,5-di-tert-butyl-4-hydroxyphenylpropionamide)] (β -form) and aqueous dispersion comprising the new crystal modifications.
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- Mixture of substances containing compounds with vinyl groups and stabilizers
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A mixture contains one or more vinyl-containing compounds as component (A) and, as a further component, a stabilizer (B) which contains one or more readily volatile nitroxyl compounds as component (b1), one or more sparingly volatile nitroxyl compounds as component (b2), if required one or more aromatic nitro compounds as component (b3) and, if required, one or more iron compounds as component (b4).Stabilizers (B) contain the components (b1) and (b2), (b1) and (b2) and (b3), (b1) and (b2) and (b4), and (b1), (b2), (b3) and (b4), and the premature polymerization of vinyl-containing compounds during their purification or distillation is inhibited by a process in which a stabilizer (B) is added or the components of stabilizer (B) are added as individual substances or in at least two groups of the components.
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- Process for the preparation of substituted hydroxyhydrocinnamate esters
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The transesterification of substituted lower alkyl hydroxyhydrocinnamates with a higher alcohol or a polyol is greatly facilitated by the use of a trace amount of a tin catalyst. In many cases, the amount of the catalyst is so small that it is unnecessary to remove it from the final product by distillation of said product.
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- Process for the production of ester compounds
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In producing ester compound useful as an antioxidant for organic materials which are represented by the formula: STR1 wherein R1 and R2 are the same or different and represent hydrogen or straight or branched chain alkyl radicals containing 1-8 carbon atoms, Z is an organic radical derived from an n-hydroxy alcohol, and n denotes an integer of 1 to 4, by transesterification, monoalkyltin compounds are used as a catalyst, whereby the ester compounds can be produced with high quality and in high yields.
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- Process for preparing organic esters and amides and catalyst system therefor
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Disclosed is a process for the preparation of organic esters and amides by reacting (a) a 5 to 60 mole % excess of an ester of (substituted-4-hydroxyphenyl) alkanoic acid with (b) (i) a C4 -C20 aliphatic alcohol or thioether alcohol having one or more hydroxyl groups or (ii) an amine of the formula, (R"')2 N(CH2)n R"" wherein R"' is hydrogen, C1-7 alkyl, C5-12 cycloalkyl, or C6-12 aryl, provided that one R"' is hydrogen, and R"" is hydrogen or N(R"')2 wherein R"' is a defined above, in the presence of a catalyst system comprising a basic inorganic compound and a polar aprotic organic compound. The process provides higher yields of the desired product, shorter reaction times, and reduces the production of undesirable side-products.
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- Method of producing tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyloxymethyl]methane
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A method of producing tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyloxymethyl]methane by ester exchange between a 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid alkyl ester and pentaerythritol in the presence of a basic catalyst, which comprises carrying out the reaction in the presence of bis[2,2,2-tris(hydroxymethyl)ethoxylmethane. According to the method of the invention, tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyloxymethyl]methane can be obtained in high yields and in high purity without using an excessively large amount of a 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid alkyl ester which is an expensive compound, while controlling the formation of the byproduct to a minimum level.
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- Process for the preparation of a hydroxyphenylcarboxylate
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Pentaerythrityl tetrakis-[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] is prepared by transesterifying a lower alkyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate with pentaerythritol in the presence of a basic catalyst, without addition of an inert solvent and in a 15 to 50% excess of lower alkyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate over the stoichiometric amount of 4 moles per 1 mole of pentaerythritol. An extremely good yield of pure crystalline product is obtained by the process of the invention.
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- Isocyanuric acid ester stabilizer
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An isocyanuric acid derivative useful as a stabilizer for organic substances, which is represented by the general formula STR1 wherein A represents STR2 R being an alkyl, cycloalkyl, aryl or aralkyl group having 1 to 8 carbon atoms; a process for preparing same; organic substances stabilized with same; and a method of stabilizing an organic substance.
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- Stabilizer for synthetic resins
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Synthetic resins, particularly polyolefins, are markedly improved in their resistances to heat and oxidation by the incorporation of a 2-methyl-4-t-butyl-5-hydroxyphenylalkanoic acid ester alone or in combination with a thioether-type antioxidant represented by the general formula STR1 wherein R represents an alkyl group of 12 to 20 carbon atoms, or by the general formula STR2 wherein R represents an alkyl group of 4 to 20 carbon atoms.
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- Process for the production of hydroxyalkylphenyl derivatives
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An improved process for the production of hydroxyalkylphenyl derivatives, especially esters and amides containing hydroxyalkylphenyl groups is disclosed, which process comprises gradually adding methyl acrylate, in the presence of an alkaline catalyst, to the alkyl substituted phenolic compound, and adding to the resultant reaction mixture a suitable alcohol or amine, optionally in the presence of a second catalyst which is different from the first catalyst. The improved process results in good yields and in a reduction of undesirable by-products while avoiding isolation of the intermediates.
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- Process for the production of hydroxyalkylphenyl derivatives
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An improved process for the production of hydroxyalkylphenyl derivatives, especially esters containing hydroxyalkylphenyl groups is disclosed, which process comprises gradually adding methyl acrylate, in the presence of an alkaline catalyst, to the alkyl substituted phenolic compound and a suitable alcohol. The improved process results in good yields and in a reduction of undesirable by-products while avoiding isolation of the intermediates.
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