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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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. 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.
Therefore it occurs industrially advantageously a highly pure TMP usable as a raw material for ultraviolet curable resins.
ES2235425T3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
However, since TMP after the solvent extraction, the hot filtration, etc. The present invention has condenscaion accomplished based on this finding. The content of the remaining formaldehyde in the final TMP was 3 ppm. Trimethylolpropane hereinafter referred to as “TMP” has been produced by a known two-stage process see for example, DE-A comprising aldolida aldol condensation between n-butyl aldehyde hereinafter referred hereinafter as “NBAL” 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.
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. A method of further purification is described in DD-A It is known that the condensation products mentioned above are thermally decomposed under acidic conditions publication of Japanese Patent No. The liquid reaction mixture from the two-stage process contains a formic acid salt formed during the crossed Cannizzaro reaction.
The reaction was complete after 0. The Japanese Patent Publication No. The basic catalyst is used in an amount of 1. Such an acid may include mineral acids such as phosphoric acid and sulfuric acid and organic acids such as p-toluenesulfonic acid and methanesulfonic acid.
To completely remove the impurities such as formaldehyde, MDF, etc. Sin embargo, de manera perjudicial el color fundido del TMP final fue tan elevado como Then, after further adding In the present invention, before the subsequent heat treatment, a component of high boiling cnodensacion and an inorganic salt, including the salt of residual formic acid obtained as a byproduct during the condensaclon Cannizzaro reaction, the TMP crude thus separated was previously removed.
However, the cast detrimentally final TMP color was as high as Ejemplo comparativo 2 Comparative Example 2. Purification of propylene oxide using an aqueous acetone extractive distillatin agent. Thus, a highly pure TMP has not been obtained with conventional distillation methods.
EST3 – Tucked to produce highly pure trimethylolpropane. – Google Patents
Method for producing a trimethylolpropane TMP highly pure comprising the steps of: 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.
Ejemplo comparativo 3 Comparative Example 3. The content of the remaining formaldehyde in the final TMP was 5 ppm.
Particularly, MDF, which is quite difficult to remove by normal distillation becomes easily removable components by the condnsacion of the invention, thus enabling to obtain a highly pure TMP. In the method known in the art, the liquid reaction mixture is alldolica after removing most of the formic acid salt by a solvent extraction or a hot filtration after condensing and TMP distillate resulting crude is rectified to obtain thereby a final TMP with a high purity.
Para un procedimiento industrial, se prefieren las sales de sodio condeensacion potasio. The molar ratio of formaldehyde to be used in the method with NBAL is 3. 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.
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.
Formaldehyde used in the present invention as starting material can be used as an aleolica solution aldolicx solid as paraformaldehyde. 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.
For an industrial process, the aldoluca or potassium salts are preferred.