Method for preparing isosorbide
A technology of isosorbide and sorbitol, applied in the field of preparation of isosorbide, can solve the problems of high production cost, low catalytic activity, increased production cost and the like, and achieves the effects of low corrosiveness, good catalytic performance and cost saving
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[0027] A preparation method of isosorbide, comprising the steps of:
[0028] [1] heating and melting solid sorbitol in a reactor to obtain a melt;
[0029] [2] Add SO to the melt obtained in step [1] 4 2- / ZrO 2 -Al 2 o 3 Immobilized acid catalyst;
[0030] [3] After step [2], the reactor is heated and depressurized, and the sorbitol in the melt undergoes a dehydration reaction to obtain isosorbide.
[0031] preferred, SO 4 2- / ZrO 2 -Al 2 o 3 The immobilized acid is prepared by co-precipitation method, sol-gel method or solvent-free grinding method.
[0032] Further preferably, the co-precipitation method includes the following steps: dissolving a certain amount of aluminum salt and zirconium salt in deionized water, adding 20%-28% ammonia water dropwise during the stirring process until the pH value of the system reaches 9-11 and co-precipitation occurs, Then filter the solution, dry the obtained precipitate at 100-120°C for 24h, soak the dried precipitate in an ...
Embodiment 1
[0039] The catalyst of this embodiment adopts co-precipitation method to prepare SO 4 2- / ZrO 2 -Al 2 o 3 catalyst. 0.103g of Al 2 (SO 4 ) 3 and 3.22 g of ZrOCl 2 ·8H 2 O was dissolved in 50ml deionized water, and 25%-28% ammonia water was added dropwise during the stirring process until the pH value of the system was 9-11, and co-precipitation occurred. The filtered sample was dried at 110°C for 24 hours, and the dried sample was soaked in an appropriate amount of 0.5 M in sulfuric acid solution, centrifuged after 5h, dried at 110°C for 24h, and calcined at 550°C in air for 5h to obtain SO with an Al / Zr molar ratio of 0.06 4 2- / ZrO 2 -Al 2 o 3 .
Embodiment 2
[0041] The catalyst of this embodiment adopts sol-gel method to prepare SO 4 2- / ZrO 2 -Al 2 o 3 catalyst. Add 20.2g of 37% hydrochloric acid to 100g of deionized water, add 5.99g of zirconium n-propoxide (70% n-butanol solution) and 0.157g of aluminum isopropoxide to the solution under stirring, and continue stirring After 5 hours, transfer to a polytetrafluoroethylene-lined hydrothermal kettle, place at 100°C for 24 hours, filter and wash to obtain a white precipitate, immerse 1g of the dried white precipitate in 15ml of 0.5M ammonium bisulfate solution, Centrifuge after 5 hours, dry at 120°C, and then calcinate at 550°C in air for 5 hours to obtain SO with an Al / Zr molar ratio of 0.06. 4 2- / ZrO 2 -Al 2 o 3 .
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