Method for preparing anhydrous sugar alcohol
An anhydrous sugar alcohol and hydrogenated sugar technology, which is applied in the preparation of organic compounds, organic chemistry methods, chemical instruments and methods, etc., can solve the problems of high catalyst cost, low conversion rate, low distillation and refining yield, etc. The effect of low rate, low cost, and improved color characteristics
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[0013] [Step (1)] The method for producing anhydrous sugar alcohol of the present invention includes the step of subjecting hydrogenated sugar to a dehydration reaction to convert it into anhydrous sugar alcohol.
[0014] The hydrogenated sugar (hydrogenated sugar) is generally also called a sugar alcohol (sugar alcohol), and means a compound obtained by adding hydrogen to a reducing terminal group of sugar. Hydrogenated sugars are classified into tetitol, pentitol, hexitol and heptitol according to the number of carbons (the number of carbons is 4, 5, 6 and 7, respectively). Among them, hexitols having 6 carbons include sorbitol, mannitol, iditol, galactitol, and the like. Sorbitol and mannitol are particularly potent substances.
[0015] The "anhydrosugar alcohol" mentioned in this specification means any substance obtained by removing one or more water molecules from the original internal structure of the hydrogenated sugar in one or more steps by any means.
[0016] In t...
Embodiment 1
[0052] Put 1,200g of sorbitol powder (D-sorbitol, SAMYANG GENEX Co., Ltd.) into a 4-port glass reactor with a stirrer, heat up to 110°C to melt, then drop into 12g of concentrated sulfuric acid (German Shan Chemical, 95%) and 7.2 g of methanesulfonic acid (Sigma, 70%), the temperature of the reaction mixture was raised to about 135°C. Maintaining this temperature, a dehydration reaction was carried out for 4 hours under a vacuum condition of 40 torr, thereby converting the starting material sorbitol into anhydrous sugar alcohol, ie isosorbide. Afterwards, reactant temperature is down to 110 ℃, in reaction result liquid, add the 50% sodium hydroxide solution of about 31.2g (Santa pure medicine ( )) to neutralize.
[0053] The neutralized anhydrous sugar alcohol is distilled at 180° C. under a vacuum below 5 torr using a thin-film distiller. The purity of the obtained anhydrous sugar alcohol distillate was 97.5%.
[0054] The obtained distillate was placed in a jacketed re...
Embodiment 2
[0058] After the anhydrous sugar alcohol converted liquid obtained in Example 1 was distilled for the first time at 180° C. under 5 torr, the obtained distillate (purity 97.5%) was subjected to the second distillation at 150° C. under 1 torr. second distillation. At this point the purity of the distillate was 98.5%. The secondary distillate (purity: 98.5%) was purified in the same order as in Example 1, in the order of crystallization, decolorization, cationic ion exchange resin treatment, and anionic ion exchange resin treatment. The final purity of the obtained anhydrosugar alcohol was 99.8%.
[0059] The ion content, pH, electrical conductivity, and YI value of the finally refined anhydrous sugar alcohol were analyzed and evaluated in the same way as in Example 1. The analysis results are shown in Table 1 below.
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