Simple preparation of expanded mesoporous silicon dioxide and dissolution promoting application of expanded mesoporous silicon dioxide

A mesoporous silica and silicon dioxide technology, applied in the direction of silica and silicon oxide, can solve the problems of low bioavailability of carvedilol, strong lipophilicity of carvedilol, complex synthesis process, etc. Achieve the effect of short cycle, large specific surface area and simple synthesis process

Inactive Publication Date: 2015-04-22
CHINA PHARM UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102992329A prepares urea-formaldehyde resin-silicon oxide composite microspheres, and then soaks and calcines the mesoporous silica particles with a specific surface area of ​​only 500m 2 /g, the reaction time is 20h, and the process is relatively complicated
Chinese patent CN102295291A adopts branch modification method to prepar

Method used

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  • Simple preparation of expanded mesoporous silicon dioxide and dissolution promoting application of expanded mesoporous silicon dioxide
  • Simple preparation of expanded mesoporous silicon dioxide and dissolution promoting application of expanded mesoporous silicon dioxide
  • Simple preparation of expanded mesoporous silicon dioxide and dissolution promoting application of expanded mesoporous silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Preparation of expanded mesoporous silica particles

[0029] (1) 0.2g of dodecyltrimethylammonium bromide and 0.35g of cetyltrimethylammonium bromide are dissolved in 200ml deionized water to form a transparent solution; 0.2g of octane is dissolved in 6ml Octane ethanol solution in ethanol.

[0030] (2) The above two solutions were mixed and ultrasonicated for 20 minutes, and then 0.3 g of sodium hydroxide was added; then 5 g of tetraethyl orthosilicate was slowly added dropwise under the condition of stirring at 80°C.

[0031] (3) React for 120 minutes under stirring at 80°C to obtain white silica emulsion; then stop stirring, filter and wash to obtain silica containing surfactant.

[0032] (4) Place the above silicon dioxide in a hydrochloric acid / ethanol solution to reflux for 3 hours, filter, wash and dry to obtain a pore-expanding silicon dioxide product with a large surface area.

Embodiment 2

[0033] Example 2: Preparation of expanded mesoporous silica particles

[0034] (1) 0.5 g of cetyltrimethylammonium bromide was dissolved in 150 ml of deionized water to form a transparent solution; 0.3 g of octane was dissolved in 8 ml of ethanol to obtain an octane ethanol solution.

[0035] (2) The above two solutions were mixed and ultrasonicated for 20 minutes, and then 0.3 g of sodium hydroxide was added; then 5 g of tetraethyl orthosilicate was slowly added dropwise under the condition of stirring at 80°C.

[0036] (3) React for 120 minutes under stirring at 80° C. to obtain white silica emulsion; then stop stirring, filter and wash to obtain silica containing surfactant.

[0037] (4) Place the above silicon dioxide in a hydrochloric acid / ethanol solution to reflux for 3 hours, filter, wash and dry to obtain a pore-expanding silicon dioxide product with a large surface area.

Embodiment 3

[0038] Example 3: Preparation of expanded mesoporous silica particles

[0039] (1) 0.6 g of cetyltrimethylammonium bromide was dissolved in 300 ml of deionized water to form a transparent solution; 0.5 g of decane was dissolved in 10 ml of ethanol to prepare a decane ethanol solution.

[0040] (2) The above two solutions were mixed and ultrasonicated for 20 minutes, and then 0.48 g of sodium hydroxide was added; then 5.6 g of tetraethyl orthosilicate was slowly added dropwise under the condition of stirring at 80°C.

[0041] (3) React for 120 minutes under stirring at 80° C. to obtain white silica emulsion; then stop stirring, filter and wash to obtain silica containing surfactant.

[0042] (4) Place the above silicon dioxide in a hydrochloric acid / ethanol solution to reflux for 3 hours, filter, wash and dry to obtain a pore-expanding silicon dioxide product with a large surface area.

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Abstract

The invention discloses a simple synthetic method of expanded mesoporous silicon dioxide with a large specific surface area and a dissolution promoting application of expanded mesoporous silicon dioxide on an insoluble drug carvedilol. The method comprises the following steps: firstly dissolving a template in deionized water, dissolving a pore-enlarging agent in ethanol, then mixing the two solutions, adding sodium hydroxide and a silicon source into the mixed solution at 80 DEG C and filtering the reaction liquid and washing the filter cake after reaction for two hours; and finally, putting the filter cake in a hydrochloric acid/ethanol solution for refluxing for 3 hours to obtain an expanded silicon dioxide product with the large specific surface area. The preparation method is easy to operate, simple in process, mild in reaction and low in cost. The prepared expanded mesoporous silicon dioxide is in a mono-dispersive spherical shape, the specific surface area reaches up to 1234.4m<2>/g and the pore diameter is 3.7nm. Finally, the mesoporous silicon dioxide and carvedilol are used for preparing a solid dispersion, and dissolution of the medicinal raw material carvedilol is obviously improved, so that the dissolution rate of carvedilol within 15 minutes reaches near 80%.

Description

technical field [0001] This patent relates to a simple preparation method of expanded mesoporous silica particles with a large specific surface area and its application to promote dissolution of the insoluble drug carvedilol. Background technique [0002] According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), porous materials are divided into three categories according to the pore size range: micropores less than 2nm; mesopores from 2 to 50nm; mesopores greater than 50nm For the macropore (macropore). Since Mobil Corporation developed the M41S material in 1992, ordered mesoporous materials have appeared on the stage as a new material. Because it has excellent characteristics that other materials do not have, especially its large specific surface area, pore volume, pore size, good stability, and abundant hydroxyl groups on the surface, it has good hydrophilicity and low toxicity. Good compatibility and other properties make it have bro...

Claims

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Application Information

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IPC IPC(8): C01B33/18
Inventor 王柏王虹
Owner CHINA PHARM UNIV
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