CN106744995B - A kind of high efficiency preparation method of the mesoporous silica particles with efficient coagulation function - Google Patents
A kind of high efficiency preparation method of the mesoporous silica particles with efficient coagulation function Download PDFInfo
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- CN106744995B CN106744995B CN201710142560.4A CN201710142560A CN106744995B CN 106744995 B CN106744995 B CN 106744995B CN 201710142560 A CN201710142560 A CN 201710142560A CN 106744995 B CN106744995 B CN 106744995B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The invention discloses a kind of high efficiency preparation methods of mesoporous silica particles with efficient coagulation function, comprising the following steps: a) ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution or ammonia spirit, by solation, gelation forms wet gel to solution again；B) wet gel and forming agent are added to pelletizer, obtain base grain；C) it is dried the base grain to obtain the mesoporous silica particles.Method of the invention, cost of material substantially reduce, and eliminate pollution dust, need not move through the xerogel stage, the manufacturing cycle of product is obviously shortened, and is improved the utilization rate of equipment while being reduced time cost.
Description
Technical field
The invention belongs to biomaterial for medical purpose fields, specifically, being a kind of mesoporous two with efficient coagulation function
The high efficiency preparation method of silicon oxide particle.
Background technique
Mesoporous silica particles, due to assigning particle outstanding absorption property with high-specific surface area and porosity,
The good biocompatibility of silica makes mesoporous silica particles become the preferred of hemostatic material simultaneously.But conventional preparation
All order mesoporous nano grade silica particles are made first with template in silica dioxide granule, then using nanometer powder as original
Material, cooperation granulating aid prepare mesoporous silica particles, and production environment receives great pollution to high production cost simultaneously.
Without using template, the speed that colloidal sol forms gel is very slow, and the reaction time is up to 120-170 hours or so, so
Conventional method all uses template first, so that colloidal sol quickly forms gel, gel process only needs 3 hours, while in dioxy
SiClx surface forms orderly meso-hole structure；But the price of organic formwork agent is very high, so that the cost of industrialization improves, and burns
Knot can not exclusively, and the residual of organic matter can reduce the biocompatibility of material；Secondly conventional method is from silicon source to silica
Grain, has an intermediate product nano grade silica particles: nanometer titanium dioxide Silica hydrogel is made from silicon source, gel drying obtains two
Silica xerogels, then xerogel is ground into nano grade silica particles, then nano grade silica particles and granulation are helped
Agent mixing granulation, powder itself and seriously polluted to operating environment with the mixing of granulating aid.
Therefore, it is still necessary to provide a kind of preparation method of environment amenable mesoporous silica particles for this field.
Summary of the invention
The purpose of the present invention is to provide a kind of environment amenable mesoporous silica particles with hemostatic function
High efficiency preparation method.
The first aspect of the present invention provides a kind of preparation side of mesoporous silica particles with efficient coagulation function
Method, which is characterized in that the preparation method comprises the following steps:
A) ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution or ammonia spirit, by solation, gelation is formed solution again
Wet gel；
B) wet gel and forming agent are added to pelletizer, obtain base grain；
C) it is dried the base grain to obtain the mesoporous silica particles.
In another preferred example, ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution, reaction terminates to obtain wet gel.
In another preferred example, ethyl orthosilicate is dissolved in ammonia spirit, reaction terminates addition aqueous hydrochloric acid solution and obtains
Wet gel.
In another preferred example, ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution, reaction terminates addition ammonia spirit and obtains
Wet gel.
In another preferred example, the concentration of the aqueous hydrochloric acid solution is 1-10vol%.
In another preferred example, the pH of the aqueous hydrochloric acid solution is 0.5-6, preferably 1-4.
In another preferred example, the concentration of the ammonia spirit is 1-10vol%.
In another preferred example, the pH of the ammonia spirit is 7-13, preferably 10-12.
In another preferred example, controlled at 20-80 DEG C in the step a), preferably 30-60 DEG C.
In another preferred example, in the step a), in 80-500 revs/min of preferable 100-200 revs/min of stirring 2-15
Hour, by solation, gelation forms wet gel to solution again.
In another preferred example, the method also includes by step a '), wet gel prepared by step a) is at 50-80 DEG C
It is dried 2-10 hours in baking oven, makes the water-holding capacity 200%-1000% of the wet gel, preferably 200%-800%, then again
Carry out step b).
In another preferred example, the forming agent is oxycellulose, oxidized regenerated cellulose, methylcellulose, carboxylic first
The combination of one or more of base cellulose, cellulose acetate, cellulose, diatomite.
It in another preferred example, is 10:1-10:8 according to xerogel and forming agent weight ratio, preferable 10:2-10:6 will be wet
Gel and forming agent are added to pelletizer.
In another preferred example, the wet gel and the forming agent are added in pelletizer (also referred to as granulator), are controlled
500-3000 revs/min of mixing speed, by strip molding (revolution is 500-1000 revs/min), cutting (turns the wet soft material after stirring
Number be 500-3500 revs/min) and round as a ball process obtain silica base grain.
In another preferred example, in the step c), the base grain is calcined in Muffle furnace and obtains mesoporous silicon oxide
Particle.Such as 300-800 DEG C calcining 0.5-3 hours.
In another preferred example, it in the step c), dries the base grain to obtain mesoporous silica particles in baking oven.
Such as 40-70 DEG C drying 2-7 hours.
In another preferred example, it in the step c), is lyophilized the base grain to obtain meso-porous titanium dioxide in freeze drier
Silicon particle.It is such as lyophilized 2-10 hours.
Method of the invention, the process route of the conventional mesoporous silica particles preparation of Optimal improvements, production cost drop
It is low, production environment optimization.The template of removal conventional method needs first, so that cost of material substantially reduces；Secondly it removes dry
Gel is directly pelletized with wet gel to the process for being crushed to powder and pelletizing again, eliminates the pollution dust of granulation early period；
Optimization technique of the third from wet gel to granulation, needs not move through the xerogel stage, and the manufacturing cycle of product is obviously shortened, and improves
The utilization rate of equipment reduces time cost simultaneously.
It should be understood that above-mentioned each technical characteristic of the invention and having in below (eg embodiment) within the scope of the present invention
It can be combined with each other between each technical characteristic of body description, to form a new or preferred technical solution.As space is limited, exist
This no longer tires out one by one states.
Detailed description of the invention
Fig. 1 is the SEM picture of mesoporous silica particles.
Fig. 2 is the SEM picture of mesoporous silica particles.
Specific embodiment
Present inventor develops a kind of new and effective meso-porous titanium dioxide by depth studying extensively for the first time
The preparation method of silicon particle, method of the invention do not need to greatly reduce products material cost by template；And in silicon source
After hydrolytic polymerization, the material of gel state is direct plungeed into the preparation that pelletizer carries out silica dioxide granule, needs not move through dry powder
The dry-mixed and wet mixing step after pelletizer is added, eliminates pollution of the dust to operating environment；Further, since material is from gel
State is directly entered pelletizer, needs not move through the xerogel stage, and the manufacturing cycle of product is obviously shortened, and improves the benefit of equipment
Time cost is reduced simultaneously with rate.On this basis, the present invention is completed.
Preparation method
The invention discloses a kind of efficient preparation process roads of novel mesoporous silica particles with hemostatic function
Line.
Specific preparation section includes preparation and grain forming and the drying steps of wet gel.
Gel preparation: ethyl orthosilicate being dissolved in 1-10% hydrochloric acid/ammonia aqueous solution, system pH 1-12, is controlled
Temperature processed at 30-60 DEG C, 100-200 revs/min stirring 2-15 hours, by solation, gelation forms gel to solution again, will
Gel dries 2-10 hours in 50-80 DEG C of baking oven, controls the water-holding capacity of gel in 200-800%.
Grain forming: according to the water-holding capacity of wet gel, determining forming agent dosage, and wet gel and forming agent are added to granulation
Machine；500-3000 revs/min of mixing speed of control, the wet soft material after stirring are formed by strip, and cutting and round as a ball process obtain two
Silica base grain.
Dry: by wet base grain, calcining/baking oven drying/freeze drier is lyophilized in Muffle furnace, obtains mesoporous silicon oxide
Particle.
In an of the invention preferred embodiment, preparation method of the invention the following steps are included:
Ethyl orthosilicate is dissolved in 1-10% hydrochloric acid/ammonia aqueous solution, control temperature is at 30-60 DEG C, 100-200
Rev/min stirring 2-15 hour, solution by solation again gelation formation gel；
Gel-like product is added directly into pelletizer, the granulation of 20-100% (ratio of auxiliary agent silica) is added
Auxiliary agent stirring；
Wet soft material is formed by strip, and cutting and round as a ball process obtain silica base grain；
Wet base grain is calcined 0-3 hours at 300-500 DEG C in Muffle furnace, or in baking 3-7 hours of 40-70 DEG C of baking oven, or
It is lyophilized 2-10 hours in freeze drier, obtains mesoporous silica particles.
The feature that the features described above or embodiment that the present invention mentions are mentioned can be in any combination.Disclosed in this case specification
All features can be used in combination with any composition form, each feature disclosed in specification, can by it is any provide it is identical,
The alternative characteristics of impartial or similar purpose replace.Therefore except there is special instruction, revealed feature is only impartial or similar spy
The general example of sign.
The invention has the beneficial effects that:
(1) cost of material is low, and production cost reduces by 60%；
(2) pollution of the dust to operating environment in existing method is eliminated, without dust in production process, has purified production ring
Border；
(3) manufacturing cycle of product is obviously shortened, and single batch of production cycle shortens 48 hours, is shortened 67%, is improved equipment
Utilization rate reduce time cost simultaneously.
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to conventional strip
Part or according to the normal condition proposed by manufacturer.Unless otherwise stated, otherwise percentage and number are weight percent and weight
Number.
Unless otherwise defined, it anticipates known to all professional and scientific terms as used herein and one skilled in the art
Justice is identical.In addition, any method similar to or equal to what is recorded and material can be applied to the method for the present invention.Wen Zhong
The preferred implement methods and materials are for illustrative purposes only.
Embodiment 1:
The aqueous hydrochloric acid solution 280mL of configuration 3%, stirs to clarify, pH value 2-4, the positive silicic acid second of 18.37mL is added dropwise
Ester TEOS, with 200 revs/min of stirring 2h, 30mL ammonium hydroxide is added after reaction and continues to stir 1min, sample is collected by filtration by 60 DEG C
Product obtain initial state wet gel；Initial state wet gel is placed in 50 DEG C of baking ovens and is heated 1 hour, so that the water content of wet gel is
400% or so.
Wet gel and cellulose acetate (according to weight ratio: gel (dry)/forming agent=10:4) are added to the granulator,
2000 revs/min of stirring 30min adjust and control 3000 revs/min of revolving speed that item processed starches 800 revs/min and grain-cutter, obtain titanium dioxide
Silicon wet granular；By silica wet granular through 600 DEG C high-temperature roasting 3 hours, obtain silica dioxide granule.
The SEM of silica dioxide granule schemes as shown in Figure 1, pore diameter range 6-9nm, is mesoporous silica particles.
Embodiment 2:
Ammonia aqueous solution 250mL, the pH value 10-12 of configuration 5%, are added dropwise 16mL TEOS, 30 DEG C, with 150 turns/
50mL hydrochloric acid is added after reaction and continues to stir 2min, sample is collected by filtration, obtains original wet gel by minute stirring 3h；It will
Original wet gel is placed in microwave experiment furnace and heats 20min, obtains the wet gel that water content is 600% or so.
Wet gel and diatomite (according to weight ratio: gel (dry)/diatomite=10:6) are added to the granulator, 1000
Rev/min stirring 60min adjusts and controls item processed and starch 500 revs/min and 1500 revs/min of grain-cutter, obtains silica wet granular；
60 DEG C of silica wet granular baking oven are dried 3 hours, silica dioxide granule is obtained.
Through detecting, pore diameter range 8-11nm is mesoporous silica particles.
Embodiment 3:
It configures in 300mL aqueous hydrochloric acid solution, stirs to clarify, pH value 1-3, be added dropwise 20mL TEOS, 30 DEG C, with
100 revs/min of stirring 15h, are collected by filtration sample, obtain wet gel；
Wet gel and cellulose (according to weight ratio: gel (dry)/cellulose=10:2) are added to the granulator, 2500
Rev/min stirring 20min, adjusts and controls 2000 revs/min of revolving speed that item processed starches 600 revs/min and grain-cutter, obtain silica
Wet granular；Silica wet granular is lyophilized 4 hours, silica dioxide granule is obtained.
The SEM of silica dioxide granule schemes as shown in Fig. 2, pore diameter range 3-5nm, is mesoporous silica particles.
All references mentioned in the present invention is incorporated herein by reference, independent just as each document
It is incorporated as with reference to such.In addition, it should also be understood that, after reading the above teachings of the present invention, those skilled in the art can
To make various changes or modifications to the present invention, such equivalent forms equally fall within model defined by the application the appended claims
It encloses.
Claims (11)
1. a kind of preparation method of the mesoporous silica particles with efficient coagulation function, which is characterized in that the preparation side
Method the following steps are included:
A) ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution or ammonia spirit, solution by solation again gelation formed it is wet
Gel；
B) wet gel and forming agent are added to pelletizer, obtain base grain；
C) it is dried the base grain to obtain the mesoporous silica particles；
Wherein, the concentration of the aqueous hydrochloric acid solution is 1-10 vol%；The pH of the aqueous hydrochloric acid solution is 0.5-6；
The concentration of the ammonia spirit is 1-10 vol%；The pH of the ammonia spirit is 7-13；
Controlled at 20-80 DEG C in the step a)；
In the step a), 80-500 revs/min stirring 2-15 hours, solution by solation again gelation formed it is wet solidifying
Glue；
The method also includes step a '), the step a) wet gel prepared is dried 2-10 hours in 50-80 DEG C of baking oven, makes institute
The water-holding capacity for stating wet gel is 200%-1000%, then carries out step b) again；
The forming agent is the combination of one or both of cellulose, diatomite；
Wet gel and forming agent are added to pelletizer for 10:1-10:8 according to xerogel and forming agent weight ratio；
The wet gel and the forming agent are added in pelletizer, 500-3000 revs/min of mixing speed of control, wet after stirring
Soft material is formed by strip, and cutting and round as a ball process obtain base grain, and the strip molding revolution is 500-1000 revs/min, described
Cutting revolution is 500-3500 revs/min；
In the step c), the base grain is calcined in Muffle furnace, baking oven dries or is lyophilized to obtain in freeze drier mesoporous
Silica dioxide granule.
2. preparation method as described in claim 1, which is characterized in that controlled at 30-60 DEG C in the step a).
3. preparation method as described in claim 1, which is characterized in that in the step a), stirred at 100-200 revs/min
2-15 hours, by solation, gelation formed wet gel to solution again.
4. preparation method as described in claim 1, which is characterized in that the method also includes step a '), it prepared by step a)
Wet gel dried 2-10 hours in 50-80 DEG C of baking oven, make the water-holding capacity 200%-800% of the wet gel, then carry out again
Step b).
5. preparation method as described in claim 1, which is characterized in that ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution, is reacted
End obtains wet gel；Or
Ethyl orthosilicate is dissolved in ammonia spirit, reaction terminates addition aqueous hydrochloric acid solution and obtains wet gel；Or
Ethyl orthosilicate is dissolved in aqueous hydrochloric acid solution, reaction terminates addition ammonia spirit and obtains wet gel.
6. preparation method as described in claim 1, which is characterized in that according to xerogel and forming agent weight ratio be 10:2-10:
Wet gel and forming agent are added to pelletizer by 6.
7. preparation method as described in claim 1, which is characterized in that in the step c), by the base grain in Muffle furnace
Mesoporous silica particles are obtained within calcining 0.5-3 hours at 300-800 DEG C.
8. preparation method as described in claim 1, which is characterized in that in the step c), the base grain is existed in an oven
40-70 DEG C obtains mesoporous silica particles in drying 2-7 hours.
9. preparation method as described in claim 1, which is characterized in that in the step c), the base grain is being freeze-dried
Machine is lyophilized 2-10 hours and obtains mesoporous silica particles.
10. preparation method as described in claim 1, which is characterized in that the cellulose is oxycellulose, Methyl cellulose
Element, carboxymethyl cellulose or cellulose acetate.
11. preparation method as claimed in claim 10, which is characterized in that the oxycellulose is oxidized regenerated cellulose.
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| CN112320806B (en) * | 2020-10-22 | 2022-02-18 | 辽宁科技学院 | Pyrolysis preparation equipment for mesoporous silica composite |
| CN113521379A (en) * | 2021-07-12 | 2021-10-22 | 重庆大清海德生物技术有限公司 | Preparation method of large-wound chitosan hemostatic particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970090A (en) * | 2006-09-14 | 2007-05-30 | 华东理工大学 | Nanometer mesoporous silicon based xerogel hemostatic material and its preparing method and use |
| CN104147633A (en) * | 2014-08-08 | 2014-11-19 | 华东理工大学 | Mesoporous hemostatic particles having antibacterial properties and their preparation method and use |
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| US20080081014A1 (en) * | 2006-10-02 | 2008-04-03 | Korea Institute Of Energy Research | Rapid preparation process of aerogel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970090A (en) * | 2006-09-14 | 2007-05-30 | 华东理工大学 | Nanometer mesoporous silicon based xerogel hemostatic material and its preparing method and use |
| CN104147633A (en) * | 2014-08-08 | 2014-11-19 | 华东理工大学 | Mesoporous hemostatic particles having antibacterial properties and their preparation method and use |
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