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Method for preparing hydroxypropyl-beta-cyclodextrin by catalysis of starch microsphere supported calcium hydroxides

A technology of calcium hydroxide and starch microspheres, which is applied in the field of catalyzing the preparation of hydroxypropyl-β-cyclodextrin by calcium hydroxide supported on starch microspheres, can solve the problems such as the intractability of alkali catalysts, and achieves a suitable degree of substitution and a fluffy feeling. Moderate, high-purity effects

Inactive Publication Date: 2012-08-15
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for the preparation of hydroxypropyl-β-cyclodextrin catalyzed by calcium hydroxide loaded on starch microspheres, which can overcome the disadvantages of difficult handling of alkali catalysts in the traditional production process of hydroxypropyl-β-cyclodextrin , but does not affect the purity and yield of the product, it is a production method of hydroxypropyl-β-cyclodextrin with simple process and low cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 1) First, add 100L deionized water and 100g calcium hydroxide to the reaction equipment, stir for 0.5 hours, then add 4kg of porous starch microspheres, control the stirring speed to 300r / min, stir and react at room temperature for 3 hours, filter, The filter cake was rinsed three times with deionized water to obtain porous starch microsphere-loaded calcium hydroxide catalyst;

[0013] 2) Next, add β-cyclodextrin, 5% catalyst of β-cyclodextrin mass in reaction equipment, and add reaction solvent water by the mass ratio of β-cyclodextrin: water=1:8, stir to obtain mixture;

[0014] 3) Then, fill the mixed solution with a pressure of 3Mpa at 25°C, control the temperature of the reaction system at 25°C, add propylene oxide dropwise according to the molar ratio of β-cyclodextrin:propylene oxide=1:7, and control the rate of addition , the dropwise addition was completed in 5 hours;

[0015] 4) Finally, keep the reaction at 25°C for 36 hours. After the reaction is completed...

Embodiment 2

[0017] 1) First, add 100L deionized water and 160g calcium hydroxide to the reaction equipment, stir for 1 hour, then add 2kg of porous starch microspheres, control the stirring speed to 100r / min, stir and react at room temperature for 1 hour, filter, The filter cake was rinsed three times with deionized water to obtain porous starch microsphere-loaded calcium hydroxide catalyst;

[0018] 2) Next, add β-cyclodextrin, 3% catalyst of β-cyclodextrin quality in reaction equipment, and add reaction solvent water by the mass ratio of β-cyclodextrin: water=1: 10, stir to obtain mixture;

[0019] 3) Then, fill the mixed solution with a pressure of 0.5Mpa at 20°C, control the temperature of the reaction system at 20°C, add propylene oxide dropwise according to the molar ratio of β-cyclodextrin:propylene oxide=1:5, and control the temperature of the dropwise Acceleration, 8 hours dropwise completed;

[0020] 4) Finally, keep the reaction at 20°C for 24 hours. After the reaction is com...

Embodiment 3

[0022] 1) First, add 100L deionized water and 140g calcium hydroxide to the reaction equipment, stir for 2 hours, then add 3kg of porous starch microspheres, control the stirring speed to 200r / min, stir and react at room temperature for 5 hours, filter, The filter cake was rinsed three times with deionized water to obtain porous starch microsphere-loaded calcium hydroxide catalyst;

[0023] 2) Next, add β-cyclodextrin, 8% catalyst of β-cyclodextrin mass in reaction equipment, and add reaction solvent water by the mass ratio of β-cyclodextrin: water=1:5, stir to obtain mixture;

[0024] 3) Then, fill the mixed solution with a pressure of 5Mpa at 15°C, control the temperature of the reaction system to be 15°C, add propylene oxide dropwise according to the molar ratio of β-cyclodextrin: propylene oxide=1:3, and control the drop rate , the dropwise addition was completed in 10 hours;

[0025] 4) Finally, keep the reaction at 15°C for 12 hours. After the reaction is completed, fi...

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Abstract

The invention discloses a method for preparing hydroxypropyl-beta-cyclodextrin by catalysis of starch microsphere supported calcium hydroxide. The method comprises the following steps of: adding beta-cyclodextrin, propylene oxide, a catalyst and water serving as a reaction solvent into reaction equipment, and reacting under certain pressure condition, wherein the reaction temperature is controlled to effectively improve the yield and the purity of the product; quickly drying the reaction product by using a spray dryer to obtain the finished product hydroxypropyl-beta-cyclodextrin. The product has the advantages of low water content, uniform particle size distribution, high whiteness, moderate substitution degree, moderate fleeciness feeling and the like, the purity of the product reaches over 99 percent, and the total yield of the reaction is over 95 percent.

Description

technical field [0001] The invention relates to a method for preparing hydroxypropyl-β-cyclodextrin, in particular to a method for preparing hydroxypropyl-β-cyclodextrin by catalyzing starch microsphere-loaded calcium hydroxide. Background technique [0002] β-cyclodextrin is composed of 7 glucose units, and the hydrogen atoms in the 2-, 3-, and 6-position hydroxyl groups of each glucose residue can be replaced by hydroxypropyl groups to obtain hydroxypropyl-β-cyclodextrin. Hydroxypropyl-β-cyclodextrin is mainly used as an excipient drug in the medical field, and its main features are: ①Increase the water solubility of insoluble drugs; ②Increase drug stability and improve drug bioavailability; ③Reduce the toxic and side effects of drugs. Hydroxypropyl-β-cyclodextrin can be used in oral drugs, injections, mucosal drug delivery systems, transdermal drug delivery systems, carriers of lipophilic targeted drugs, and can also be used as protein protectants and stabilizers. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16
Inventor 王蕾苗宗成
Owner SHAANXI UNIV OF SCI & TECH
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