Preparation method of D-mannitol alpha crystal form
A technology of mannitol and crystal form, which is applied in the field of preparation of D-mannitol alpha crystal form, can solve the problems of high energy consumption, continuous operation difficulty, product crystal form impurity and other problems of D-mannitol alpha crystal form, and achieve The effect of easy control of temperature distribution, wide range of experimental conditions and low production cost
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Embodiment 1
[0038] Precipitate preparation after embodiment 1 sea-tangle extracts iodine
[0039] S1. Take 1 kg of dried kelp and soak it with 5 kg of soaking solution for 90 minutes, then add 12 kg of tap water and continue soaking for 30 minutes to obtain the kelp soaking solution;
[0040] S2. Add calcium agent to the kelp soaking solution obtained in step S1 and adjust the pH value to 8.0, centrifuge and inflate, and take the clear solution after standing for 1 hour;
[0041] S3. Separating the supernatant obtained in step S2 for the preparation of iodine simple substance, and S2 centrifuging and inflating the supernatant to separate the remaining precipitate, that is, the precipitate after extracting iodine from kelp as a raw material for preparing the alpha crystal form of D-mannitol.
Embodiment 2
[0042] Example 2 Preparation of alpha crystal form D-mannitol from the precipitate after extracting iodine from kelp
[0043] S1. Centrifuge and filter the iodine-extracted precipitate from kelp at 4000r / min, add edible-grade ethanol of equal quality to the filter residue, stir at 100r / min for 10min, cool down to 0°C, and let stand for 18h until the crystals are precipitated to obtain a crystal solution;
[0044] S2. Centrifugally filter the crystal solution obtained in step S1 to obtain filtrate A and filter residue A, add the same quality of edible grade ethanol to filter residue A, stir at 100r / min for 10min, and stand at a constant temperature of -10°C for 6h to obtain a crystallization liquid;
[0045] S3. High-speed centrifugal filtration of the crystalline liquid obtained in step S2 to obtain filtrate B and filter residue B;
[0046] S4. Combine filtrate A and filtrate B, concentrate until the specific gravity of the filtrate is 1.2, repeat step S2 and step S3 once, com...
Embodiment 3
[0047] Example 3 Preparation of alpha crystal form D-mannitol from the precipitate after extracting iodine from kelp
[0048] S1. Centrifuge and filter the iodine-extracted precipitate from kelp at 4200r / min, add edible-grade ethanol of the same quality to the filter residue, stir at 110r / min for 100min, cool down to 3°C, and let stand for 12h until the crystals are precipitated to obtain a crystal solution;
[0049] S2. Centrifugally filter the crystal solution obtained in step S1 to obtain filtrate A and filter residue A, add the same quality of edible grade ethanol to filter residue A, stir at 110r / min for 100min, and stand at a constant temperature of -8°C for 8h to obtain a crystallization liquid;
[0050] S3. High-speed centrifugal filtration of the crystalline liquid obtained in step S2 to obtain filtrate B and filter residue B;
[0051] S4. Combine filtrate A and filtrate B, concentrate until the specific gravity of the filtrate is 1.2, repeat step S2 and step S3 once,...
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