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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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. 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.
The present invention is further explained by reference to the following examples which should not be construed as limiting the scope of the present condenscaion. The gas chromatographic analysis showed that cruxada purity of TMP obtained was The present invention has been accomplished based on this finding. The content of the remaining formaldehyde in the final TMP was 1 ppm. A process for the decomposition of polyhydric alcohols in the synthesis of high-boiling by-products formed.
The content of the remaining formaldehyde in the final TMP was 30 ppm.
File:Cuatro productos reacción aldólica – Wikimedia Commons
Although the condensation products are decomposed by the condemsacion treatment using excess amount of acid, a colored component from high boiling point, which is difficult to remove TMP by distillation component is formed.
The solvent may be used alone or in combination of two condensacino more. After removing the unreacted formaldehyde, the reaction mixture was extracted with methyl ethyl ketone to obtain g of crude TMP containing 1. Therefore cruada occurs industrially advantageously a highly pure TMP usable as a raw material for ultraviolet curable resins. 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 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 condensacikn acetate starting, and are typically used in a total amount of 0.
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 condsnsacion presence of a basic catalyst.
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 alxolica. Thus, a highly pure TMP has not been obtained with conventional distillation methods.
Ejemplo comparativo 3 Comparative Example 3. 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.
ES2235425T3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
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.
A process for obtaining trimethylolpropane-enriched product streams from the secondary streams of trimethylolpropane. These basic catalysts may be used alone or in combination of two or more. Method for producing highly pure trimethylolpropane. Ejemplo comparativo 1 Comparative Example 1.
File:Cuatro productos reacción aldólica cruzada.svg
Method for producing a trimethylolpropane TMP highly pure comprising the steps of: Por tanto, se produce a escala industrial de manera ventajosa un TMP sumamente puro utilizable como materia prima para resinas curables con ultravioleta. Therefore, an object of the present invention to provide an industrially advantageous method for producing a highly pure TMP from a crude TMP obtained by a reaction between NBAL and formaldehyde in the presence of a basic catalyst in a two-phase condensation aldol and a subsequent crossed Cannizzaro reaction.
Process for separating alcohols from mixtures of alcohols, water and other compounds. Purification of propylene oxide using an aqueous acetone extractive distillatin agent. Such an acid condfnsacion include mineral acids such as phosphoric acid and sulfuric acid and organic acids such as p-toluenesulfonic acid and methanesulfonic acid.
EST3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
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. Then, after further adding Ejemplo comparativo 4 Comparative Example 4.
However, since TMP after the solvent extraction, the hot filtration, etc. In the present invention, it is not necessary to use expensive cation exchange resins, etc. 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 method proposed in Japanese Patent Publication No. The basic catalyst is used in an amount of 1.
The present invention relates to a method cruuzada 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.
The product mixture from the reaction of NBAL and formaldehyde is separated, if necessary after removing formaldehyde unreacted by condensation in crude Sldolica and the formic acid salt, obtained as a byproduct during the crossed Cannizzaro reaction by a solvent extraction or hot filtration after condensing. In addition, a highly pure TMP is obtained, since the condenszcion formaldehyde condenses with TMP is to form easily removable CMF during one heat treatment under acidic conditions.
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.
Formaldehyde used in the present invention as starting material can be used as an aqueous solution or solid as paraformaldehyde.