Preparation method of mannitol

A technology of mannitol and water extraction, applied in the field of mannitol preparation, can solve the problems of low efficiency of glucose electrolysis, problem of raw material sources, poor quality of mannitol, etc., achieve good decolorization effect, low cost, and good crystallization effect Effect

Inactive Publication Date: 2010-08-25
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, mannitol is usually chemically synthesized, but there are many problems: the glucose electrolysis method has low efficiency, high energy consumption, and low purity; the products of the reduction method of polysaccharides have isomerization problems, and the cost is high and the pur

Method used

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  • Preparation method of mannitol

Examples

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Example Embodiment

Example 1

Take 1 kg of the residue of the triterpene acid extracted from Ligustrum lucidum leaves, add 15L of deionized water, heat at 75°C for 1.5 hours, and filter to obtain the extract. The extraction liquid is decolorized by a polyalum hollow fiber ultrafiltration membrane system with a molecular weight cut-off of 20,000, and the permeate is collected. The permeate was heated and concentrated to a relative density of 1.30 to 1.32, and allowed to stand to cool and crystallize to obtain 52 g of crude crystals. Add 52ml of deionized water to the crude crystals, boil for 5 minutes and then cool to crystallize. Recrystallize the precipitated crystals twice under the same conditions. Wash the crystals with 6L ether and dry at 80°C to obtain 3.8g of mannitol. The purity is 98.5% by HPLC. .

Example Embodiment

Example 2

Take 1 kg of the triterpene acid residue from Ligustrum lucidum leaves, add 16L of deionized water, heat at 80°C for 1.5 hours, and filter to obtain the extract. The extraction liquid is decolorized by a polyalum hollow fiber ultrafiltration membrane system with a molecular weight cut-off of 20,000, and the permeate is collected. The permeate was heated and concentrated to a relative density of 1.30 to 1.32, and allowed to stand to cool and crystallize to obtain 54 g of crude crystals. Add 60ml of deionized water to the crude crystals, boil for 5 minutes and then let cool to crystallize. The precipitated crystals are recrystallized twice under the same conditions. The crystals are washed with 7L ether and dried at 90°C to obtain 3.9g of mannitol. The purity is 98.6% by HPLC. .

Example Embodiment

Example 3

Take 1 kg of the residue of the triterpene acid extracted from Ligustrum lucidum leaves, add 18L of deionized water, heat at 75°C for 2 hours, and filter to obtain the extract. The extraction liquid is decolorized by a polyalum hollow fiber ultrafiltration membrane system with a molecular weight cut-off of 20,000, and the permeate is collected. The permeate was heated and concentrated to a relative density of 1.30 to 1.32, and allowed to stand to cool and crystallize to obtain 53 g of crude crystals. Add 55ml of deionized water to the crude crystals, boil for 5 minutes and then let cool to crystallize. Recrystallize the precipitated crystals twice under the same conditions. The crystals are washed with 8L ether and dried at 80°C to obtain 3.8g of mannitol. The purity is 99.2% by HPLC. .

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Abstract

The invention relates to a preparation method of mannitol. The technique comprises the following steps: extracting glossy privet leaf of triterpenic acid as a raw material, using 15-20 times (V/W) of deionized water to extract for 1.5-2 hours, carrying out ultrafiltration on extracting solution by an ultrafiltration membrane system with molecular weight cut off of 20000, heating and concentrating permeate till the relative density is 1.30-1.32, standing and crystallizing, using the deionized water to dissolve coarse crystal, boiling for 5 minutes, filtering with heat, recrystallizing for three times, using ether to clean, and drying at the temperature of 80-90 DEG C to obtain a product. The technique has simple operation, lower cost and higher purity and is beneficial to large-scale production operation.

Description

technical field The invention relates to a method for preparing mannitol, in particular to a method for extracting mannitol from privet leaf extraction residue. Background technique Mannitol, also known as D-mannitol and wood honey, is an isomer of sorbitol, both of which are hexavalent alcohols. English name: Mannitol Molecular formula: C 6 h 14 o 6 Molecular weight: 182.17 White needle crystal. The melting point is 166°C, the relative density is 1.52, 1.489 (20°C), and the boiling point is 290-295°C (467kPa). 1g of this product is soluble in about 5.5ml of water (about 18%, 25°C), 83ml of alcohol, more soluble in hot water, soluble in pyridine and aniline, and insoluble in ether. The aqueous solution is alkaline. With the chemical properties of polyols, it can be esterified, etherified, oxidized, and dehydrated. It is the only non-hygroscopic crystal among polyols. In the prior art, mannitol is usually chemically synthesized, but there are many problems: the...

Claims

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Application Information

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IPC IPC(8): C07C31/26C07C29/76
Inventor 李法庆张翼刘东锋
Owner 苏州宝泽堂医药科技有限公司
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