Synthesis,charaterization And Crystal Structures Of Spiroglycol With Large Particle Size And High Purify

Isobutylaldehyde is byproduct of octyl alcohol. Although it can be used synthetic fine chemical products as organic chemical materials, it is not well to its additional rate. Spiroglycol is an important secondly product of isobutylaldehyde, and it is a new polycol. It is widely used by its particular structure. It is necessary to make a good technical way which fit the condition of our country and quickly make the civil chemical product progress ability because the market of spiroglycol is mainly abroad. It is very significant not only in the widely used developing, but also in academic. It find a good way to the used of isobutylaldehyde.Now spiroglycol is synthesized in second steps at abroad. First HPA is made in alkaline catalyst by isobutylaldehyde and formaldehyde, and second SPG is made in acid by hydroxypivalaldehyde and pentaerythritol. The optimum condition is made by effect under the contrast in the reaction pressure, temperature, time, the mole ratio of materials which in two steps. The optimum condition of synthetic hydroxypivalaldehyde in sodium carbonate : the reaction temperature is 66℃, the mole ratio is 1:1, the reaction time is 5h, the amount of catalyst is 0.029mol/mol HCHO. The reaction of synthetic HPA is second grades reaction kinetics model, its reaction rate equilibrium is:The optimum condition of synthetic SPG which in a 36wt% hydrochloric acid is made by the Orthogonal test : the reaction temperature is 75℃, the mole ratio of pentaerythritol and hydroxypivalaldehyde is 1:2.5, the amount of hydrochloric acid is 0.26mol/molPE, the reaction time is 4.5h, the amount of water is 3kg/mol PE. Developed a new way at the same time, seed crystals are added to the reaction system and the mother liquid is reused in the next reaction. It reduced the environmental load, proved the produce efficiency and had a good industrial prospect.At the end, the structure of hydroxypivalaldehyde has been characterized by IR and GC-MS spectra. The structure of spiroglycol has been characlerized by IR and HNMR, spectra, and obtains the spiroglycol crystal in synthetic process, which crystal structures have also been determined by X-ray single crystal diffraction.