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.
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The final product quality is adversely affected by the remaining formaldehyde even in a small amount. The method proposed in Japanese Patent Publication No. Deactivation is carried out by adding the acid to the crude TMP in an amount 0.
Masters and doctoral program in Chemical Sciences
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.
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 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 in a total amount of 0.
In the following examples and comparative examples, the content of the remaining formaldehyde in the final TMP product was determined by acetylacetone method, and the color cast APHA color pattern obtained according to JIS K document 6. The content of the remaining formaldehyde in the final TMP was 3 ppm. The Japanese Patent Publication No.
Recently, TMP has come to be widely used and particularly in the use as raw material for ultraviolet curable resins, TMP presenting a higher purity to previously reached require. Ejemplo comparativo 1 Comparative Example 1.
The product mixture from the 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 content of the remaining formaldehyde in the final TMP was 30 ppm. Formaldehyde used in the present invention as starting material can be used as an aqueous solution or solid as paraformaldehyde.
A method of further purification is described in DD-A To minimize the occurrence of byproducts and increase selectivity of the objective TMP, preferred set the amount of the basic catalyst according to the reaction conditions. The present invention is further explained by reference to the following examples which should not be construed aldplica limiting the scope of the present invention.
Trimethylolpropane hereinafter referred to as “TMP” has been produced by a known two-stage process see for example, DE-A comprising an aldol condensation between n-butyl aldehyde hereinafter referred hereinafter as cruzxda and formaldehyde in the presence of a basic catalyst and a subsequent crosslinking reaction between the aldol condensation product and formaldehyde in a basic catalyst Cannizzaro.
ES2235425T3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
Ejemplo comparativo 3 Comparative Example 3. Method for producing highly pure trimethylolpropane. Ejemplo comparativo 2 Comparative Example 2. The reaction was complete after 0. In addition, a highly pure TMP is obtained, since the remaining formaldehyde condenses with TMP is to form easily removable CMF during one heat treatment under acidic conditions. In the present invention, before the subsequent heat treatment, a component of high boiling point and an inorganic salt, including the salt of residual formic acid obtained as a byproduct during the crossed Cannizzaro reaction, the TMP crude thus separated was previously removed.
After removing the component and high boiling inorganic salt of crude TMP, the resultant TMP distillate is subjected to a heat treatment under acidic conditions. These basic catalysts may be used alone or in combination of two or more. In the present invention, it is not necessary to use expensive cation exchange resins, etc.
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.
Purification of propylene oxide using an aqueous acetone extractive distillatin agent.
File:Cuatro productos reacción aldólica cruzada.svg
However, the cast detrimentally final TMP color was as high as Method for producing a trimethylolpropane TMP highly pure comprising the steps of: 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 by distillation. However, since TMP after the solvent extraction, the hot filtration, etc.
In the present invention, as described above, after first removing cndensacion inorganic salt such as sodium formate, and the component of high boiling the crude TMP, the treated TMP is subjected to heat treatment under acidic conditions. Thus, a highly pure TMP has not been obtained with conventional distillation methods. 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.
Recientemente, el TMP ha empezado a ser ampliamente utilizado y particularmente en el uso como materia prima para resinas curables con ultravioleta, presentando el TMP una pureza superior a la que antes se ha llegado a requerir.
The basic catalyst is used in an amount of 1. The present invention relates to a method of producing trimethylolpropane which is useful as a raw material for polyester resins, alkyd resins, dondensacion resins, polycarbonate resins, plasticizers, lubricating oils, surfactants, basis for cosmetics, reactive monomers, etc.
Although the condensation products are decomposed by the heat treatment using excess amount of acid, a colored component from high boiling point, which is condennsacion to remove TMP by distillation component is formed.
Sin embargo, de manera perjudicial el color fundido del TMP final fue tan elevado como 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. A process for obtaining trimethylolpropane-enriched product streams from the secondary streams of trimethylolpropane.
Particularly, MDF, which is quite difficult cruaada remove by normal distillation becomes easily removable components by the treatment of the invention, thus enabling to obtain a highly pure TMP.
The present invention relates to a method of purifying a crude TMP obtained by an aldol condensation and a subsequent crossed Cannizzaro reaction of NBAL of formaldehyde in the presence of a basic catalyst. Para un procedimiento industrial, se prefieren las sales de sodio o potasio. Process for separating alcohols from mixtures of alcohols, water and other compounds.
The purity of TMP obtained was Method for producing a highly pure trimethylolpropane according to claim 1, 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.