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A high-efficiency preparation method of mesoporous silica particles with high-efficiency blood coagulation function

A technology of mesoporous silica and coagulation function, applied in the field of medical biomaterials, can solve the problems of high production cost, high price, increased cost, etc., and achieve the effects of eliminating polluting dust, shortening the preparation period and reducing the production cost.

Active Publication Date: 2019-05-21
苏州佰济生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the conventional preparation of silica particles, the ordered mesoporous nano-silica powder is first prepared by using a template agent, and then the nano-powder is used as a raw material to prepare mesoporous silica particles with granulation aids. The production cost is high and the production environment is high. has been heavily polluted
[0003] Without the use of a template, the sol forms a gel very slowly, and the reaction time is as long as 120-170 hours. Therefore, the conventional method first uses a template to allow the sol to quickly form a gel. The gel process only takes 3 hours. An ordered mesoporous structure is formed on the surface of silica; however, the price of the organic template is very high, which increases the cost of industrialization, and the sintering will be incomplete, and the residue of organic matter will reduce the biocompatibility of the material; secondly, the conventional method starts from From silicon source to silica particles, there is an intermediate product nano-silica powder: nano-silica gel is prepared from silicon source, the gel is dried to obtain silica xerogel, and then the xerogel is ground into nano Silica powder, and then mix nano-silica powder and granulation aids for granulation, the powder itself and the mixing with granulation aids will seriously pollute the operating environment

Method used

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  • A high-efficiency preparation method of mesoporous silica particles with high-efficiency blood coagulation function
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preparation example Construction

[0033] The specific preparation process includes the preparation of wet gel and particle forming and drying steps.

[0034] Gel preparation: Dissolve ethyl orthosilicate in 1-10% hydrochloric acid / ammonia aqueous solution, the pH value of the system is 1-12, control the temperature at 30-60°C, stir at 100-200 rpm for 2-15 hours, The solution is gelled and then gelled to form a gel, and the gel is baked in an oven at 50-80° C. for 2-10 hours, and the water holding capacity of the gel is controlled at 200-800%.

[0035] Granule forming: Determine the amount of forming agent according to the water holding capacity of the wet gel, add the wet gel and forming agent to the granulator; control the stirring speed at 500-3000 rpm, and the wet soft material after stirring is formed into strips, The cutting and spheronizing process obtains the silica pellets.

[0036] Drying: Calcining the wet pellets in a muffle furnace / drying in an oven / lyophilizing in a freeze dryer to obtain mesopor...

Embodiment 1

[0050]Prepare 280mL of 3% hydrochloric acid aqueous solution, stir until clear, the pH value is 2-4, add 18.37mL tetraethyl orthosilicate TEOS dropwise, stir at 60°C and 200 rpm for 2h, add 30mL ammonia water after the reaction and continue stirring After 1 min, the sample was collected by filtration to obtain the initial wet gel; the initial wet gel was heated in an oven at 50° C. for 1 hour, so that the water content of the wet gel was about 400%.

[0051] Add the wet gel and cellulose acetate (according to the weight ratio: gel (dry) / forming agent=10:4) into the granulator, stir at 2000 rpm for 30 minutes, adjust and control the bar pulping at 800 rpm and cut The rotational speed of the particle knife is 3000 rpm to obtain wet silicon dioxide particles; the wet silicon dioxide particles are calcined at 600° C. for 3 hours to obtain silicon dioxide particles.

[0052] SEM images of silica particles figure 1 As shown, the pore size ranges from 6-9nm, which are mesoporous sil...

Embodiment 2

[0054] Prepare 250mL of 5% aqueous ammonia solution, the pH value is 10-12, add 16mL TEOS dropwise, stir at 30°C and 150 rpm for 3h, add 50mL hydrochloric acid and continue stirring for 2min after the reaction, collect the sample by filtration, and obtain the initial wet condensation Gel; heat the initial wet gel in a microwave oven for 20 minutes to obtain a wet gel with a water content of about 600%.

[0055] Add the wet gel and diatomaceous earth (according to the weight ratio: gel (dry) / diatomite=10:6) into the granulator, stir at 1000 rpm for 60 minutes, adjust and control the bar making at 500 rpm and The dicing knife was set at 1500 rpm to obtain wet silica granules; the wet silica granules were baked in an oven at 60° C. for 3 hours to obtain silica granules.

[0056] After testing, the pore diameter ranges from 8-11nm, which is mesoporous silica particles.

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Abstract

The invention discloses an efficient preparation method of mesoporous silica particles with an efficient blood coagulation function. The method comprises the following steps of (1) dissolving tetraethylortho silicate into a hydrochloric acid water solution or an ammonia-water solution and carrying out solating and gelation on the solution to form wet gel; (b) adding the wet gel and a forming agent to a granulator to obtain blank particles; and (c) drying the blank particles to obtain the mesoporous silica particles. According to the method, the raw material cost is greatly reduced, the polluting dust is eliminated, a gel drying stage is not needed, the preparation cycle of a product is obviously shortened, and the time cost is reduced while the utilization rate of equipment is improved.

Description

technical field [0001] The invention belongs to the field of medical biomaterials, in particular to a high-efficiency preparation method of mesoporous silicon dioxide particles with high-efficiency blood coagulation function. Background technique [0002] Mesoporous silica particles endow particles with excellent adsorption properties due to their high specific surface area and porosity, and the good biocompatibility of silica makes mesoporous silica particles the first choice for hemostatic materials. However, in the conventional preparation of silica particles, the ordered mesoporous nano-silica powder is first prepared by using a template agent, and then the nano-powder is used as a raw material to prepare mesoporous silica particles with granulation aids. The production cost is high and the production environment is high. was greatly polluted. [0003] Without the use of a template, the sol forms a gel very slowly, and the reaction time is as long as 120-170 hours. Ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12
CPCC01B33/12C01P2004/03C01P2006/17
Inventor 洪华刘昌胜袁媛周华溢王成伟
Owner 苏州佰济生物科技有限公司
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