Preparation technique of isosorbide
A technology of isosorbide and preparation process, which is applied in the field of pharmacy, can solve the problems of high cost, low conversion rate, carbonization of raw materials, etc., and achieve the effect of improving utilization rate, avoiding the disadvantage of high energy consumption, and excellent quality
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Embodiment 1
[0024] (1) Dehydration reaction
[0025] Weigh 250kg of solid sorbitol, melt it in a pressure reactor at 120°C, add 30% by weight of the catalyst obtained by mixing perfluorosulfonic acid resin and carbon-based palladium (mixed 4:1 by weight), at 150°C The reaction was stirred for 4 hours, and a hydrogen pressure of 0.2 MPa was always maintained in the reactor during the reaction.
[0026] The light transmittance of the obtained reaction solution was 86%, and the purity was 75.3% as detected by HPLC.
[0027] (2) Neutralization and decolorization
[0028] Pure water was added to dilute the reaction solution to a Brix of 19%. Use calcium carbonate suspension to adjust the pH value to neutral; add 7.5% activated carbon based on dry matter and stir at 75°C for 30 minutes to decolorize, and the transmittance of the reaction solution obtained by filtration is 96%.
[0029] (3) Electrodialysis desalination
[0030] After the treatment in step (2), the conductivity was 17600 μs / c...
Embodiment 2
[0040] (1) Dehydration reaction
[0041] Weigh 250kg of solid sorbitol, melt it in a pressure reactor at 110°C, add 5% by weight of perfluorosulfonic acid resin and carbon-based palladium mixed catalyst (6:1 by weight), at 150°C The reaction was stirred for 7 hours, and a hydrogen pressure of 0.3 MPa was always maintained in the reactor during the reaction.
[0042] The light transmittance of the obtained reaction solution was 89%, and the purity was 72.8% as detected by HPLC.
[0043] (2) Neutralization and decolorization
[0044] Pure water was added to dilute the reaction solution until the Brix was 20%. Use calcium carbonate suspension to adjust the pH value to neutral; add 5% activated carbon based on dry matter and stir at 75°C for 40 minutes to decolorize, and the transmittance of the reaction solution obtained by filtration is 98%.
[0045] (3) Electrodialysis desalination
[0046] After the treatment in step (2), the conductivity was 15300 μs / cm, and after further...
Embodiment 3
[0056] (1) Dehydration reaction
[0057] Weigh 250kg of solid sorbitol, melt it in a pressure reactor at 130°C, add 15% by weight of a catalyst obtained by mixing perfluorosulfonic acid resin and carbon-based palladium (8:1 by weight), at 150°C The reaction was stirred for 2 hours, and a hydrogen pressure of 0.2 MPa was always maintained in the reactor during the reaction.
[0058] The light transmittance of the obtained reaction solution was 82%, and the purity was 75.6% as detected by HPLC.
[0059] (2) Neutralization and decolorization
[0060] Pure water was added to dilute the reaction solution to a Brix of 18%. Use calcium carbonate suspension to adjust the pH value to neutral; add 10% activated carbon based on dry matter and stir at 75°C for 20 minutes to decolorize, and the transmittance of the reaction solution obtained by filtration is 99%.
[0061] (3) Electrodialysis desalination
[0062] After the treatment in step (2), the conductivity was 20200 μs / cm, and afte...
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