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Preparation method of high-purity 1,4-sorbitan

A sorbitan, high-purity technology, applied in the field of preparation of cyclic ethers, can solve problems such as not seen

Active Publication Date: 2013-03-06
NANJING WELL BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] So far, the domestic and foreign markets have not seen the supply of 1,4-sorbitol products

Method used

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  • Preparation method of high-purity 1,4-sorbitan
  • Preparation method of high-purity 1,4-sorbitan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1400g sorbitol in a 2000ml three-necked bottle, vacuumize (water pump), gauge pressure-0.01MPa, heat up, temperature rises from room temperature to 120°C, and dehydrate for 2 hours in total. Cool down to 90°C, add 50g of phosphorous acid, slowly heat up under reduced pressure for dehydration, keep the vacuum at -0.01MPa, and the maximum temperature is 142°C for 6 hours, add 1400ml of water to dilute after cooling, and use hydrogen Calcium oxide is neutralized, and the generated calcium salts are removed by filtration. The aqueous solution was decolorized by adding 28 g of activated carbon, the activated carbon was removed by filtration, and the filtrate was concentrated under reduced pressure to obtain 842.5 g of sorbitan crude product, which was analyzed by liquid chromatography with a content of 73.74% and a yield of 70%.

Embodiment 2～6

[0033] Identical to embodiment 1, but suitable variation is arranged, and experimental result is listed in the following table:

[0034]

Embodiment 7

[0036] Mix 800 g of the 1,4-sorbitol crude product obtained in Example 1 with 320 g of methanol, heat to 60° C., mix well, stir, gradually cool down to 20° C., precipitate crystals, and filter to obtain 520 g of primary crystallization crude product, the content Increase to 87%; 520g primary crystallization crude product, mixes with 156g methanol, crystallizes by above same method, obtains 312g secondary crystallization crude product, content improves to 94%; 312g secondary crystallization crude product, mixes with 94g methanol, by above same method Method for crystallization to obtain 150 g of tertiary crystallization product, HPLC analysis, product content 99.23%.

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Abstract

The invention discloses a preparation method of high-purity 1,4-sorbitan, which is characterized by taking D-sorbitol as a raw material through dewatering twice and three times of crystallization. The method comprises the following steps of: (1) adding polyatomic alcohol in a reaction vessel; (2) stirring, heating and decompressing for removing free water; (3) cooling down and adding an acidic catalyst; (4) stirring, heating and decompressing for dehydrating a molecule of water; (5) neutralizing and filtering for separating the catalyst; (6) decolorizing; (7) carrying out crystallization for three times in lower alcohol to prepare the 1,4-sorbitan with more than 99% of content. The preparation method fills up the blank of 1,4-sorbitan industrial production technique; the prepared 1,4-sorbitan can be used for synthesizing high-purity surfactants, such as Span, Tween, sorbitan fatty acid ester or polysorbate and the like; and the polysorbate-80 synthesized by the prepared 1,4-sorbitan can satisfy the standard of injection-level pharmaceutic adjuvant.

Description

technical field [0001] The invention relates to a preparation method of a cyclic ether, and the cyclic ether is 1,4-sorbitol. Industrial sorbitol undergoes secondary dehydration to first produce 1,4-sorbitol, and then use crystallization to produce high-purity 1,4-sorbitol. The solvent used for crystallization is methanol or other lower alcohols. technical background [0002] 1,4-Sorbitol, commonly known as sorbitan, is a product obtained by losing a molecule of water in the sorbitol molecule, and is a cyclic ether compound. There are four hydroxyl groups in the 1,4-sorbitol molecule, which can undergo etherification and esterification reactions, for example, ethoxylation with ethylene oxide to generate polyoxyethylene sorbitan ether, and polyoxyethylene sorbitan ether Esterification of fatty acids to synthesize Span compounds. These compounds all have excellent surface activity, so 1,4-sorbitol has a wide range of applications in the surfactant industry. [0003] The mol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/20
Inventor 吴仁荣高正松贾建国周霞娟
Owner NANJING WELL BIOCHEM
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