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D-sorbitol crystalline solid and preparation method thereof

A technology of crystalline solid and sorbitol, applied in the field of D-sorbitol crystalline solid and preparation thereof, can solve the problems of difficult filtration, viscous crystal slurry, low crystallinity, etc., and achieves simple and easy-to-control operating conditions and good crystal habit. , the effect of high crystallinity

Active Publication Date: 2011-11-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] In addition to the above operating restrictions, it has been verified by experiments that the products obtained by various methods in the literature generally have disadvantages such as low crystallinity, viscous crystal slurry, and difficult filtration.

Method used

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  • D-sorbitol crystalline solid and preparation method thereof
  • D-sorbitol crystalline solid and preparation method thereof
  • D-sorbitol crystalline solid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 20g of Gamma-type D-sorbitol solid into 100g of N,N-dimethylformamide, heat up to 30°C to dissolve completely, then cool the solution down to 5°C, and separate the resulting solid-liquid suspension by suction filtration , and the resulting solid was dried. The micrograph of the sorbitol product after drying is as Figure 5 As shown, the product is a rod-shaped crystal, and the crystal habit is better than that of Gamma-type granular aggregates.

[0031] The dried product was analyzed and determined, and the PXRD pattern had characteristic peaks at diffraction angles 2θ=7.4, 12.8, 14.8, 19.8, 22.6, 24.0, 26.0, 27.1, 32.7, 38.2 and 39.6 degrees, and DSC had a peak at 75.0°C Melting endothermic peaks, FTIR spectrum at 3376, 2931, 1635, 1418, 1316, 1258, 1196, 1105, 1092, 1050, 1017, 938, 894, 874, 644, 588, 506 and 480cm -1 There are characteristic peaks at 1248, 1132, 1096, 1060, 1020, 962, 941, 876, 775, 742, 645, 595, 505, 478, 412, 354 and 250cm -1 There are cha...

Embodiment 2

[0033] Add 50g of F-type D-sorbitol solid mixture into 100g of N,N-dimethylacetamide, heat up to 70°C to dissolve completely, cool down to 30°C at a cooling rate of 5°C / h, and filter the solid Liquid suspension, the suction filtration time is 6min, which saves more than half than the suction filtration time (greater than 30min) of other methods for D-sorbitol crystal preparation. The obtained solid was dried at 30° C. and a vacuum of 0.1 MPa. After drying, the sorbitol product is a rod-shaped crystal.

[0034] The dried product was analyzed and determined, and the PXRD pattern had characteristic peaks at diffraction angles 2θ=7.3, 12.8, 14.8, 19.7, 22.4, 23.8, 25.9, 27.0, 32.9, 38.0 and 39.5 degrees, and DSC had a peak at 74.0°C Melting endothermic peaks, FTIR spectrum at 3374, 2928, 1631, 1415, 1315, 1260, 1195, 1105, 1094, 1049, 1016, 940, 893, 873, 643, 589, 507 and 478cm -1 There are characteristic peaks at 1249, 1131, 1094, 1059, 1018, 961, 942, 878, 774, 741, 647, 597,...

Embodiment 3

[0036] Add 30g of Gamma-type D-sorbitol solid into 100g of formamide, heat up to 70°C, stir to dissolve completely, cool down to 20°C at a cooling rate of 8°C / h, and filter the solid-liquid suspension with suction. 10min. The obtained solid was dried at 40° C. and a vacuum of 0.09 MPa. After drying, the sorbitol product is a rod-shaped crystal.

[0037] The dried product was analyzed and determined, and the PXRD pattern had characteristic peaks at diffraction angles 2θ=7.1, 12.6, 14.6, 19.8, 22.4, 23.8, 25.8, 26.9, 32.8, 38.0 and 39.3 degrees, and DSC had a peak at 73.4°C. Melting endothermic peaks, FTIR spectrum at 3375, 2930, 1635, 1416, 1317, 1257, 1197, 1106, 1091, 1050, 1015, 937, 892, 871, 645, 589, 508 and 479cm -1 There are characteristic peaks at 1247, 1131, 1094, 1059, 1019, 961, 941, 878, 774, 740, 645, 595, 504, 477, 411, 354 and 249cm in the Raman spectrum -1 There are characteristic peaks, and the product is F-type D-sorbitol. The characteristic peaks of its ...

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Abstract

The invention relates to a D-sorbitol crystalline solid and a preparation method thereof. The crystal type is defined as Type F, which is defined by X-ray powder diffraction spectrum, DSC (Differential Scanning Calorimetry) characteristic endothermic peak, infrared spectrum and Raman spectrum. The preparation method comprises the following steps: dissolving any type of D-sorbitol in an amide solvent to form a solution, wherein the temperature is 30-70 DEG C, and the mass ratio of the amide solvent to the D-sorbitol is (2-5):1; cooling the solution to 5-30 DEG C; separating the solid-liquid suspension; and drying the collected solid to obtain the F-type crystal product of D-sorbitol. The crystal type product of D-sorbitol has the advantages of high degree of crystallization, good crystal habit and high crystal slurry filtering rate; and the operating conditions of the preparation method are simple and easy to control.

Description

field of invention [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a D-sorbitol crystalline solid and a preparation method thereof. Background of the invention [0002] Sorbitol is D-sorbitol, the full name is sorbitol, also known as herbal tea alcohol, rose alcohol, etc., the chemical name is 1, 2, 3, 4, 5, 6-hexyl alcohol, and the English name is D-sorbitol. Also known as D-glucitol, its chemical structure is as follows: [0003] [0004] Sorbitol has a sweet taste, its sweetness is about 60% of that of sucrose, but its calories are only one third (2.6 calories per gram). It is non-cariogenic and beneficial for people with diabetes. Sorbitol has been used safely in processed foods, but excessive use can have diarrheal effects. In addition to its sweet taste, sorbitol is also a good humectant and thickener for the production of cosmetics, confectionery, bakery and chocolate. The moisture stabil...

Claims

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Application Information

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IPC IPC(8): C07C31/26C07C29/78
Inventor 郝红勋王艳蕾王静康尹秋响侯宝红王永莉张美景龚俊波鲍颖高俊彦
Owner TIANJIN UNIV
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