como nucleofilo en el carbono del benzaldehído, realizando una reacción de condensación de Claisen-Schmidt (tipo de condensación aldolica cruzada). Particulares ○ Efectuar una condensación aldólica cruzada. ○ Obtener un producto de uso comercial. Diferencia entre una condensación aldólica cruzada y. Específicos Efectuar una condensación aldólica cruzada. Determinar el rendimiento de la reacción realizada y el punto fusión del producto obtenido.
|Genre:||Health and Food|
|Published (Last):||25 April 2010|
|PDF File Size:||18.30 Mb|
|ePub File Size:||13.9 Mb|
|Price:||Free* [*Free Regsitration Required]|
Process for separating alcohols from mixtures of alcohols, water and other compounds.
ES2235425T3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
A process for the decomposition of polyhydric alcohols in the alrolica of high-boiling by-products formed. The present invention relates to a method of producing trimethylolpropane which is useful as a raw material for polyester resins, alkyd resins, polyurethane resins, polycarbonate resins, plasticizers, lubricating oils, surfactants, basis for cosmetics, reactive monomers, etc.
In the present invention, as the load of distillation column is reduced, the distillation apparatus improved from the economic viewpoint with respect to the structure and operatively allowing it to produce a highly pure TMP advantageously in industrial scale.
However, since TMP after the solvent extraction, the hot filtration, etc. Ejemplo comparativo 1 Comparative Example 1.
Sin embargo, de manera perjudicial el color fundido del TMP final fue tan elevado como As a result of extensive studies in the production method of TMP to eliminate the above problems, the inventors have found that a highly pure TMP is obtained from a crude TMP by previously removing a component of high boiling point and an inorganic salt such as sodium formate, the crude TMP, heat-treating the treated TMP under acidic conditions, and purifying the heat-treated TMP by distillation, etc.
In the following examples and comparative examples, the content of the remaining formaldehyde in the final TMP product was determined by acetylacetone method, and wldolica color cast APHA color pattern obtained according to JIS K document 6.
The reaction was complete after 0. Method for producing highly pure trimethylolpropane. However, the cast detrimentally final TMP color was as high as TMP obtained by the reaction between NBAL and formaldehyde in the presence of basic catalyst in the two-stage process of the aldol condensation and the subsequent crossed Cannizzaro reaction contains the impurities hardly removable fruzada distillation. Para un procedimiento industrial, se prefieren las sales de sodio o potasio.
Without adding phosphoric acid and without subjecting to heat treatment, g of the distillate mainly comprising TMP by distillation at under a reduced pressure of Pa 1 Torr using a column with Sulzer-packed 10 theoretical stages purified. The gas chromatographic analysis condensaciion that the purity of TMP obtained was However, when TMP contains the formic acid salt and the component of high boiling condensation products are decomposed hard by heat treatment in the presence of acid even in an amount equivalent to the amount of formic acid saltleaving obtained this a highly pure TMP mode.
The present invention has been accomplished based on this finding.
Condensación de aldehídos simples by Adrian Yazan on Prezi
For aldoica, the two-phase process using sodium hydroxide is expressed by the following reaction scheme. The present invention is further explained by reference to the following examples which should not be construed as limiting the scope of condenszcion present invention. To completely remove the impurities such as formaldehyde, MDF, etc. With such heat treatment, the component hardly removable from TMP by distillation is thermally decomposed or chemically combines to form an easily removable component of TMP by distillation.
The product mixture from aldplica reaction of NBAL and formaldehyde is separated, if necessary after removing formaldehyde unreacted by condensation in crude TMP and the formic acid salt, obtained as a byproduct during the crossed Cannizzaro reaction by a solvent extraction or hot filtration after condensing.
The liquid reaction mixture from the two-stage process contains a formic acid salt formed during the crossed Cannizzaro reaction. In the present invention, it is not necessary to use expensive cation exchange resins, etc.
EST3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
TMP obtained by purification of crude TMP by akdolica method of the present invention has such a high purity as The basic catalyst is used in an amount of 1. Method for producing a trimethylolpropane TMP highly condenxacion comprising the steps of: The aldol condensation and the subsequent crossed Cannizzaro reaction may be carried out in the presence of water in an amount of 2 to 20 times by weight of NBAL.
The impurities are free formaldehyde, condensation products of TMP and formaldehyde, methanol contained in formalin starting, methanol formed during the crossed Cannizzaro reaction, condensation products of methanol, TMP and formaldehyde, etc.
Method for producing a highly pure trimethylolpropane according to claim condensacuon, wherein component removing high boiling point and the inorganic salt is carried out after deactivating sodium formate present in the crude trimethylolpropane, wherein the deactivation is carried out by means of adding an acid to crude TMP in an amount 0.
The content of the remaining formaldehyde in the final TMP was 30 ppm.
The solvent for the extraction may include ketones such as methyl ethyl ketone and methyl isobutyl ketone, aldehydes such as NBAL, also serving as material of alcohols such as isobutyl alcohol and isopropyl alcohol, and esters such as butyl acetate starting, and are typically used ocndensacion a total amount of 0. Particularly, MDF, which is quite difficult to remove by normal distillation becomes easily removable components by the treatment of the invention, thus enabling to obtain a highly pure TMP.
Ejemplo comparativo 3 Comparative Example 3.