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A kind of preparation method of mesoporous double-layer organosilicon sphere

A silicone and double-layer technology, applied in the preparation of organic compounds, medical preparations of non-active ingredients, organic chemistry, etc., can solve the problem that it cannot be used as a drug release carrier of different sizes, affects the function of silicon spheres, and cannot be completely removed Templating agent and other issues

Inactive Publication Date: 2016-11-30
高飞
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Problems solved by technology

[0008] 3. Due to the use of P85 (EO26PO39EO26) as the template agent, only alcohol / acid solution extraction cannot achieve the effect of completely removing the template agent, so the residual template agent affects the adsorption function of the silica spheres
[0010] 1. This method uses calcination to remove the surfactant, which consumes a lot of energy, has poor safety and high cost
[0011] 2. The material prepared by this method has a single channel, which cannot be used as a carrier material for the type of reaction in which the size of the reaction substrate changes greatly during the reaction, nor can it be used as a carrier for the graded release of drugs of different sizes
This also restricts the application in hierarchical reaction system, biological cascade reaction, chemical cascade reaction, and drug partial release to a certain extent.

Method used

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  • A kind of preparation method of mesoporous double-layer organosilicon sphere
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  • A kind of preparation method of mesoporous double-layer organosilicon sphere

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preparation example Construction

[0048] A preparation method of mesoporous double-layer silicone spheres, comprising the following steps:

[0049] 1) Tetraethylammonium bromide, Al(OH) 3 and Ca(OH) 2 Add in deionized water and mix evenly to obtain a mixed solution A. Ultrasonic the mixed solution A for 5 to 24 hours until it is completely uniform, then take it out, then heat it to 80-120°C and stir evenly to obtain a mixed solution B; ,

[0050] The tetraethylammonium bromide, Al(OH) 3 , Ca(OH) 2 And the molar ratio of deionized water is 0.5~0.8:0.3~0.5:0.5:3000~4000;

[0051] 2) Add ammonia water to the mixed solution B obtained in step 1), and then add 1,4-bis(triethoxysilyl)benzene dropwise at a rate of 10 drops per minute and adjust the pH to 10-13, The temperature rises to 80-100°C, and after reacting for 5-7 hours, a mixed solution C is obtained; wherein,

[0052] The molar ratio of tetraethylammonium bromide, ammonia water and 1,4-bis(triethoxysilyl)benzene is 0.5-0.8:0.01-0.03:1;

[0053] 3) Tr...

Embodiment 1

[0062] At room temperature, 0.38gTAB (tetraethylammonium bromide), 0.1gAl(OH) 3 with 0.135gCa(OH) 2 Add 150 mL of deionized water and mix evenly (mol ratio of Ca / Si=0.5). The whole system was ultrasonicated for 6 hours, and after the system was completely uniform, it was taken out, heated to 100°C and stirred evenly. Join NH 3 .H 2 After 0.01 mL, 1.0 g (2.5 mmol) of 1,4-Bis(triethoxysilyl)-benzene (1,4-bis(triethoxysilyl)benzene) was slowly added dropwise (pH=12.8). After reacting at 100°C for 5 hours, the reaction liquid was transferred to a high-pressure reactor and reacted at 110°C for 72 hours, and the solid was obtained by suction filtration. The solid was extracted with HCl-EtOH at 80 °C for 12 h. The reaction product was dried in a vacuum oven at 60° C. for 5 hours. This gave 0.82 g of a white solid.

[0063] 1.0g of compound 1 and 0.1g of Al(OH) 3 Add 5mL triethanolamine, add 0.12g CTAB and 0.08g CTAC in 100mL water once, stir for 1h, the temperature rises to 6...

Embodiment 2

[0065] At room temperature, 0.21gTAB (tetraethylammonium bromide), 0.09gAl(OH) 3 with 0.08gCa(OH) 2 Add 140 mL of deionized water and mix evenly (mol ratio of Ca / Si=0.5). The whole system was ultrasonicated for 12 hours. After the system was completely uniform, it was taken out, heated to 90°C and stirred evenly. Join NH 3 .H 2 After 0.02 mL, 0.8 g (2 mmol) of 1,4-Bis(triethoxysilyl)-benzene (1,4-bis(triethoxysilyl)benzene) was slowly added dropwise (pH=11.8). After reacting at 80° C. for 8 h, the reaction liquid was transferred to a high-pressure reactor to react at 100° C. for 3 days, and the solid was obtained by suction filtration. The solid was extracted with HCl-EtOH at 60 °C for 24 h. The product was dried in a vacuum oven at 60°C for 5 hours. This gave 0.42 g of a white solid.

[0066] 0.7g of compound 1 and 0.05g of Al(OH) 3 Add 3mL of triethanolamine, add 0.07g of CTAB and 0.04g of CTAC in 80mL of water once, stir for 1 hour, the temperature rises to 80°C, di...

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Abstract

The invention relates to a method for preparing mesoporous double-layer organic silicon balls, which includes the following steps: adding TAB (tetraethylammonium bromide), Al(OH) 3 with Ca(OH) 2 After dissolution and sonication, the temperature was raised. After adding a small amount of ammonia, the silicon source 1,4-Bis(triethoxysilyl)-benzene (1,4-bis(triethoxysilyl)benzene) was dropped to adjust the pH to alkaline. The reaction liquid is placed in the kettle at high temperature overnight to obtain the precursor product. The product obtained above is mixed with Al(OH) 3 , triethanolamine, CTAB (cetyltrimethylammonium bromide), CTAC (cetyltrimethylammonium chloride), mix evenly and then heat up, add the silicon source bistrimethoxysilylethane, react After a period of time, a white solid was obtained and extracted with HCl-EtOH to obtain the target material. The present invention prepares two different mesopores in the first shell and the second shell of the sphere respectively. The pores in the inner shell are smaller, about 2 to 4 nm, and the pores in the outer shell are larger, about 10 to 17 nm. Due to the existence of different pore sizes, different pore sizes are suitable for molecules of different sizes to enter.

Description

technical field [0001] The invention relates to a method for preparing a mesoporous double-layer organic silicon sphere. Background technique [0002] Ordered mesoporous nanomaterials are a class of heterogeneous catalyst supports with great potential for practical application. It has a high specific surface area, which provides a chance for the chemical reaction to contact the catalyst, thereby improving the reactivity; secondly, the surface of this type of material has a large number of hydroxyl groups, which provides a large number of modification sites for the modification and modification of the target catalyst. point. The third is good hydrothermal stability, which can still ensure a high degree of order under relatively strong conditions, which greatly facilitates the application of catalysts. Its four pore sizes can be adjusted, and mesoporous materials with different pore sizes can be synthesized through different templates, which solves the problem of pore limita...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J32/00B01J31/02C07C29/34C07C33/18A61K47/24
CPCA61K47/24B01J20/22B01J20/28019B01J20/28035B01J20/28054B01J31/0274C07C33/46C07C33/18C07C29/143C07C29/34B01J35/647
Inventor 高飞
Owner 高飞
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