CN113772683B - Preparation method of mesoporous silica, mesoporous silica and its application - Google Patents
Preparation method of mesoporous silica, mesoporous silica and its application Download PDFInfo
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Abstract
本发明涉及二氧化硅领域，具体涉及一种介孔二氧化硅的制备方法、介孔二氧化硅及其应用。介孔二氧化硅的制备方法包括以下步骤：将去除胞外分泌物及培养液后的硅藻藻体冻干至凝固，再将其冻干至恒重，获得硅藻粉末；采用酸溶液对硅藻粉末进行清洗，去除硅藻粉末中的有机质，获得介孔二氧化硅材料。本发明提供的介孔二氧化硅的制备方法，通过采用冻干硅藻后再酸洗的方法获得介孔二氧化硅，建立起一种纯化硅藻壳制备介孔二氧化硅的方法，从而实现快速、定量、完整地获得介孔二氧化硅，且得到的二氧化硅材料介孔均一，为介孔二氧化硅的进一步研究提供了极大的方便。
The present invention relates to the field of silica, and specifically relates to a preparation method of mesoporous silica, mesoporous silica and its application. The preparation method of mesoporous silica includes the following steps: freeze-drying the diatom algae after removing extracellular secretions and culture medium until solidification, and then freeze-drying it to constant weight to obtain diatom powder; using an acid solution to treat the silicon dioxide The algae powder is cleaned to remove organic matter in the diatom powder and obtain mesoporous silica material. The method for preparing mesoporous silica provided by the present invention obtains mesoporous silica by freeze-drying diatoms and then pickling them, and establishes a method for purifying diatom shells to prepare mesoporous silica, thereby Mesoporous silica can be obtained quickly, quantitatively and completely, and the obtained silica material has uniform mesopores, which provides great convenience for further research on mesoporous silica.
Description
Technical Field
The invention relates to the field of silicon dioxide, in particular to a preparation method of mesoporous silicon dioxide, the mesoporous silicon dioxide and application thereof.
Background
Mesoporous materials are novel materials with pore diameters between micropores and macropores. The mesoporous silica material has the characteristics of an excellent adsorption material: pore structure order, pore size distribution singleness and controllability, and mesoporous shape diversity, so that the catalyst has very important functions in the fields of adsorption separation, industrial catalysis, biomedicine, environmental protection and the like.
At present, mesoporous silica is mainly prepared by a template method, micelles are formed by self-aggregation under acidic or alkaline conditions by using different types of templates such as surfactants, block copolymers and the like, then silicon sources are added for hydrolysis to form silica which is self-assembled on the surface of the templates, and finally the templates are removed by extracting the templates or calcining to retain silica products.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect of complex process for preparing mesoporous silica by a template method in the prior art, thereby providing a preparation method of mesoporous silica, the mesoporous silica and application thereof.
The invention provides a preparation method of mesoporous silica, which comprises the following steps:
freeze-drying diatom algae body after removing extracellular secretion and culture solution to solidify, and freeze-drying the diatom algae body to constant weight to obtain diatom powder;
and cleaning the diatom powder by adopting an acid solution to remove organic matters in the diatom powder, thereby obtaining the mesoporous silica material.
Optionally, the acid solution comprises sulfuric acid and hydrogen peroxide, and the volume ratio of the sulfuric acid to the hydrogen peroxide is 7:3.
Optionally, the diatom algae is Navicula australoshetlandica sp.
Optionally, the step of cleaning the diatom powder with an acid solution comprises the following steps:
1ml of acid solution: mixing the acid solution and the diatom powder according to the proportion of (20 mg-50 mg) of the diatom powder, and performing ultrasonic dispersion and then digesting the mixture solution in a water bath at 60 ℃ until the mixture solution shows clear color;
carrying out suction filtration on the digested mixed solution to obtain a filter cake;
and (3) cleaning and freeze-drying the filter cake to obtain the mesoporous silica material.
Optionally, the suction filtration step adopts a PTFE filter membrane.
Optionally, the washing comprises the step of resuspending the filter cake with deionized water and centrifugally washing 3 times.
Optionally, the freeze-drying comprises the step of freezing the cleaned filter cake at-80 ℃ until no flowing components exist, and then freeze-drying for 12 hours.
Optionally, the diatom algae after removing extracellular secretion and culture solution is obtained according to the following steps:
the diatom algae which have been cultivated to be complete are collected by centrifugation, resuspended in deionized water and washed by centrifugation for 3 times.
The invention also provides mesoporous silica which is prepared by the preparation method according to any one of the schemes.
The invention also provides application of the mesoporous silica in hemostasis.
The technical scheme of the invention has the following advantages:
1. according to the preparation method of mesoporous silica, the mesoporous silica is obtained by adopting the method of freeze-drying diatom and then acid washing, and the method for preparing the mesoporous silica by purifying the diatom shell is established, so that the mesoporous silica is obtained rapidly, quantitatively and completely, the obtained silica material is uniform in mesopore, and great convenience is provided for further research of the mesoporous silica.
2. According to the preparation method of mesoporous silica, the dried silica powder is obtained in a freeze-drying mode, so that the original form of diatom can be kept under the dry powder state, and the phenomenon that extrusion deformation and even cracking occur among diatom bodies during drying can be avoided.
3. According to the preparation method of the mesoporous silica, the acid solution prepared by the hydrogen peroxide and the sulfuric acid according to the specific proportion is used for cleaning the diatom powder, and has strong oxidizing property, so that more hydroxyl groups on the surface of the diatom shell can be endowed while the organic matters of the diatom are fully digested, the hydrophilicity of the material is improved, the cleaned acid can be recovered, and only a small amount of hydrogen peroxide is needed to be supplemented.
4. According to the preparation method of the mesoporous silica, provided by the invention, after the filter cake is cleaned, the filter cake is still dried by adopting a freeze-drying technology, so that the obtained mesoporous silica can be ensured to have good dispersibility and complete morphology, materials adhered to a centrifuge tube are reduced, and the loss is reduced.
5. The mesoporous silica provided by the invention is prepared by adopting a specific method, and the obtained mesoporous silica is uniform in mesopore.
6. The mesoporous silica provided by the invention has the advantages of quick coagulation and good hemostatic effect when applied to hemostasis.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope image of diatom mesoporous silica in example 1 of the present invention;
FIG. 2 is a transmission scanning electron microscope image of diatom mesoporous silica in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of diatom mesoporous silica in example 2 of the present invention;
FIG. 4 is a scanning electron microscope image of diatom mesoporous silica in example 3 of the present invention;
FIG. 5 is a scanning electron microscope image of the diatom mesoporous silica of comparative example 2 of the present invention;
FIG. 6 is a scanning electron microscope image of the diatom mesoporous silica of comparative example 3 of the present invention;
FIG. 7 shows the haemostatic effect of mesoporous silica in the evaluation of the haemostatic effect of mesoporous silica according to the invention;
FIG. 8 is an in vitro clotting time results in the evaluation of the hemostatic effect of mesoporous silica according to the present invention;
FIG. 9 shows the results of coagulation test in the evaluation of the hemostatic effect of mesoporous silica according to the present invention.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment relates to a preparation method of mesoporous silica, which specifically comprises the following steps:
s1, centrifugally collecting the fully cultured diatom algae (Navicula australoshetlandica sp.), re-suspending with deionized water, centrifugally cleaning for 3 times, and removing the culture solution and extracellular secretion thereof;
s2, putting the algae obtained in the step S1 into a temperature of minus 80 ℃, freezing for 1h, transferring into a freeze vacuum dryer, and freeze-drying to constant weight to obtain diatom powder;
s3, sulfuric acid: hydrogen peroxide = 7:3, preparing an acid solution in proportion;
s4, mixing 1mL of acid solution: mixing the acid solution and the diatom powder in a triangular flask according to the proportion of 50mg of the diatom powder, transferring to an ultrasonic machine for dispersing for 5min, transferring to a water bath kettle at 60 ℃ for digestion for 30min;
s5, after digestion, transferring the mixed solution to a suction filtration device, performing suction filtration by using a PTFE filter membrane, scraping a filter cake which is the diatom mesoporous silica material, transferring the filter cake to a centrifuge tube, adding deionized water for resuspension, and centrifugally cleaning for 3 times to obtain the diatom mesoporous silica;
s6, putting the diatom mesoporous silica into a-80 ℃, freezing for 1h, transferring into a freeze vacuum dryer, and freeze-drying to obtain powder (the quality and the duration of depending on the algae powder are different, and the longest time is not more than 12 h), so as to finally obtain white diatom mesoporous silica powder which is uniformly dispersed into powder.
The embodiment can reach mesoporous silica material from diatom powder by less than 18 hours. And shooting diatom and mesoporous silica diatom shells thereof by using a scanning electron microscope and a transmission electron microscope to obtain an electron microscope photo, wherein the electron microscope photo is shown in figures 1-2, the figure 1 is a scanning electron microscope picture of the mesoporous silica diatom, and the figure 2 is a transmission scanning electron microscope picture of the mesoporous silica diatom. As can be seen from fig. 1-2, the surface of the diatom mesoporous silica has pore distribution of different pore diameters ranging from 165 to 350nm. And the holes with diameters of 6-8nm which are orderly arranged in the interior can be clearly seen by enlarging the holes with diameters of more than 100 nm. This shows that the method for cleaning the diatom shells in this embodiment can effectively remove the organic matters of diatom, and retain the complete structure and fine structure of diatom, thereby obtaining mesoporous and uniform mesoporous silica material. This reticulated substructure can greatly increase the surface area of Navicula australoshetlandica sp, which is beneficial in its use as a mesoporous biomaterial.
Example 2
This example relates to a method for preparing mesoporous silica, which differs from example 1 in that in this example, sulfuric acid in acid solution: hydrogen peroxide = 3:7.
The transmission scanning electron microscope picture of the mesoporous silica obtained in the embodiment is shown in fig. 3. As can be seen from fig. 3, the organic matter removal is not clean enough.
Example 3
This example relates to a method for preparing mesoporous silica, which differs from example 1 in that in this example, sulfuric acid in acid solution: hydrogen peroxide=5:5.
The transmission scanning electron microscope picture of the mesoporous silica obtained in the embodiment is shown in fig. 4. As can be seen from fig. 4, the diatom has been partially broken.
Comparative example 1
The comparative example relates to the preparation of a mesoporous silica material, comprising the following steps:
1. preparation of amorphous silica spheres
160mL of ethanol, isopropanol or butanol was stirred with 16mL of ammonium hydroxide and 7g of n-silanoethanol (TEOS) in a stoppered 500mL round bottom flask at room temperature for 20h. The silica microspheres were recovered and purified by centrifugation and washing with ethanol for a number of cycles and dried overnight at 70-80 ℃.
2. Hydrothermal reaction (preparation of mesoporous silica sphere)
The amorphous parent silica spheres are converted to mesoporous silica spheres using a pseudomorphic conversion reaction. Amorphous silica spheres (44 mg) dispersed in ethanol (2.53 mL) were added to a mixture of CTAB (0.05 g), water (10 mL) and NaOH (0.013 g), and stirred at room temperature for 30 minutes. The molar ratio of all components was 1 SiO2:0.18 CTAB:0.44 NaOH:750 H2O:75 EtOH. The hydrothermal reaction was carried out in a polytetrafluoroethylene-lined autoclave at 100℃for 24 hours. The product was recovered and purified by centrifugation and multiple cycles of washing with ethanol. The surfactant was removed from the mesoporous silica spheres by calcination in air at 550 ℃ for 6 hours (heating rate 1 ℃/min). The final product is expressed as HT-SiO 2 -EtOH、HT-SiO 2 -iPrOH and HT-SiO 2 BuOH, depending on the cue ballSolvents used in the synthesis.
The template method is more complicated, time-consuming and pollution-free in preparing mesoporous silica materials.
Comparative example 2
This comparative example relates to a method for preparing mesoporous silica, which is different from example 1 in that in this comparative example, the water bath temperature in step S4 is 40 ℃.
The transmission scanning electron microscope picture of the mesoporous silica obtained in this comparative example is shown in fig. 5. As can be seen from fig. 5, the organic matter removal is not clean enough.
Comparative example 3
This comparative example relates to a method for producing mesoporous silica, which is different from example 1 in that in this comparative example, the water bath temperature in step S4 is 90 ℃.
The transmission scanning electron microscope picture of the mesoporous silica obtained in this comparative example is shown in fig. 6. As can be seen from fig. 6, the diatom portion has been broken.
Mesoporous silica hemostatic Effect evaluation
1. In vitro hemolysis experiment
In vitro hemolysis experiments were performed using different concentrations of diatom shell powder. Diatom shells were dissolved in physiological saline (10 mg/ml, 5mg/ml, 2.5mg/ml, 1mg/ml, 0.5 mg/ml) and water-bath was performed at 37℃in advance. 60mL of 10% hematocrit red blood cell dispersion was added to 1mL of the diatom shell dispersion solution followed by 20mL of CaCl2 in a 37℃water bath for 1h. The solution was then centrifuged at 2000rpm/min for 5 minutes. The absorbance of the supernatant at 545nm was measured. Distilled water and physiological saline without diatom shells were used as positive and negative controls, respectively.
Calculation formula of hemolysis rate:
HR (%) = (Ds diatom shell-Dn physiological saline)/(Dp distilled water-Dn). Times.100
2. In vitro procoagulant activity of diatom shells
Taking clean test tubes, adding 10mg of diatom shell powder respectively, taking blank test tubes as negative control, taking chitosan as positive control, and setting three test tubes per concentration of each sample. The tubes were gently shaken or the powder was spread as far as possible at the bottom of the tube and preheated to 37 ℃. 0.25mL, 0.5mL, 0.75mL, 1mL, 1.25mL fresh blood and anticoagulated blood (blood: 3.8% sodium citrate = 9:1) are sequentially added to the above tubes, smoothly transferred to a 37 ℃ water bath, placed in the water bath while starting timing, the first tube is tilted once every 30s (angle is less than 30 °), the remaining two tubes are temporarily immobilized until the first tube is slowly inverted and the blood does not flow, the second and third tubes are observed in the same way until the blood in the third tube is fully coagulated, and the set of clotting times is recorded according to a stop watch. The coagulation time is up to 60min, and the coagulation is judged to be non-coagulation after exceeding. The test was repeated 6 times per sample.
The samples in each tube were washed three times with phosphate buffered saline (PBS, pH 7.4) to remove blood cells that did not adhere to the powder. Adding 2.5% glutaraldehyde solution into the washed diatom shell powder and RBC complex, and standing at room temperature for 2h to crosslink the blood cells and the diatom shell powder. Dispersing the fixed powder with alcohol, dripping on a silicon wafer, spraying gold, and taking an electron scanning microscope picture.
3. Activated partial thrombin time (aPTT) assay
100L PPP was water-bathed at 37℃for 3min, then mixed with aPTT reagent and sample (in grams) also water-bathed at 37℃for 3min, and then transferred to a fully automatic coagulation analyzer for measurement, each sample was tested 6 times, and the average was taken.
4. Prothrombin Time (PT) determination
100L of Platelet Poor Plasma (PPP) and PT reagent were mixed together and preheated at 37℃for 5min. The prepared samples were added and then transferred to a fully automatic coagulation analyzer for measurement, each sample was tested 6 times, and the average value was taken.
5. Experimental results:
(1) Rate of in vitro hemolysis
The hemolysis test was used to confirm the compatibility of the diatom shell with blood. This test measures haemolysis mainly caused by electrostatic interactions between silanol groups distributed on the surface of the diatom shell and positively charged groups of the membrane proteins. The strong affinity between silica and cell membrane weakens the integrity of erythrocytes. As the concentration of diatom shell increases, the rate of hemolysis of Red Blood Cells (RBCs) becomes substantially higher, as shown in fig. 7. To quantify the hemolysis of the diatom shells in SD rat erythrocytes, the rate of hemolysis was calculated (according to equation 1.).
D F ,D N And D P Absorbance at 545nm, for diatom shell, distilled water (negative control) and normal saline (positive control), respectively.
From FIG. 7, at 1, 2.5 and 5 mg. Mu.mL -1 Low hemolysis was found in the diatom shell, not exceeding 1.55.+ -. 0.06%. At 1 mg. Mu.mL -1 In the diatom shell, the lowest hemolysis rate is 1.18±0.22%, which can be considered as almost transparent resolution (fig. 8). Although 7.5mg mL -1 The hemolysis rate of (a) reaches 4.73+/-0.45 percent, but is still lower than 5 percent. When 10mg mL is used -1 When the diatom shell is added into the erythrocyte solution, the hemolysis rate is 5.64+/-0.39%, which is significantly higher than 1, 2.5 and 5mg/mL -1 Concentration (p)<0.001)。However, the data is still advantageous compared to that of coscinodicut sp. Diatom shell (17.76+ -1.16%, 10mg mL) -1 ) And diatomaceous earth (13.83.+ -. 0.11%,5mg mL) -1 ). The obtained results indicate that Navicula australoshetlandica sp.
(2) Results of in vitro coagulation
The hemostatic effect of the diatom shell is measured by the clotting time of whole blood in vitro. The anticoagulated blood used in this evaluation was added at 1/50V 0.025mol/L CaCl 2 Recalcification. The calcium chloride here provides the appropriate calcium ion (factor iv) into the anticoagulant, which causes the coagulation process to be activated and reacted. To compare hemostatic efficiency, the clotting time was assessed for diatom shells and chitosan suspended in different volumes of blood. Chitosan is a natural polysaccharide that is widely used as a commercial hemostatic material due to its effective hemostatic properties, biodegradability and biocompatibility. In this study we used chitosan as a positive control. According to FIG. 9, the setting time of the diatom shell and chitosan was significantly shorter than that of the blank (429.37.+ -. 12.14 s). The clotting time of the diatom shell group at a hemostatic material/blood (mg/. Mu.L) ratio of 1:100 was the shortest (134.99.+ -. 7.00 s), 1.83 times (112.32 s) and 3.18 times (294.38 s) shorter than that of chitosan, and shorter than that of the control group. When the blood volume was increased from 25. Mu.L to 125. Mu.L, the clotting time of chitosan was significantly prolonged from 181.06.+ -. 7.25 to 282.52.+ -. 3.48s, while the clotting time of diatom shells remained almost unchanged, changing from 167.37.+ -. 13.33s to 181.73.+ -. 7.60s. This indicates that the blood volume has a slight effect on the hemostatic properties of the diatom shell, showing great potential as a hemostatic material for medical use.
(3) Activated partial thromboplastin time (aPTT) and Prothrombin Time (PT)
Characterization of activated partial thromboplastin time (aPTT) and Prothrombin Time (PT) revealed a role for diatoms in the hemostatic pathway. The aPTT of the diatom shells was 44.53+ -7.78 s shorter than the control, while there was no significant change in PT (P <0.5, using SPSS analysis) (blood was 8.73+ -0.12 s; diatom shells were 8.85+ -0.37 s), as shown in FIG. 7. Shortening of aPTT means an intrinsic pathway by which diatom shells can induce blood clotting. Previous studies have shown that the highly porous, negatively charged surface of silica can activate the intrinsic pathways of blood coagulation by stimulating coagulation factors XI and XII [28,29]. The large number of negatively charged groups can be attributed to the shortened aPTT, while the nearly constant PT indicates that the diatom shell does not activate the extrinsic coagulation pathway.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (1)
1. The preparation method of the mesoporous silica is characterized by comprising the following steps of:
s1, centrifugally collecting the diatom algae Navicula australis algae cultivated to be complete,
resuspension with deionized water, centrifugal cleaning for 3 times, and removing culture solution and extracellular secretion;
s2, putting the algae obtained in the step S1 into a temperature of minus 80 ℃, freezing for 1h, transferring into a freeze vacuum dryer, and freeze-drying to constant weight to obtain diatom powder;
s3, sulfuric acid: hydrogen peroxide = 7:3 volume ratio of the prepared acid solution;
s4, mixing 1mL of acid solution: mixing the acid solution and the diatom powder in a triangular flask according to the proportion of 50mg of the diatom powder, transferring to an ultrasonic machine for dispersing for 5min, transferring to a water bath kettle at 60 ℃ for digestion for 30min;
s5, after digestion, transferring the mixed solution to a suction filtration device, performing suction filtration by using a PTFE filter membrane, scraping a filter cake which is the diatom mesoporous silica material, transferring the filter cake to a centrifuge tube, adding deionized water for resuspension, and centrifugally cleaning for 3 times to obtain the diatom mesoporous silica;
s6, putting the diatom mesoporous silica into a-80 ℃, freezing for 1h, transferring into a freeze vacuum dryer, freeze-drying to obtain powder, and finally obtaining white diatom mesoporous silica powder which is uniformly dispersed into powder, wherein the diameter of the pore is 165-350nm, enlarging pores with the diameter of more than 100nm, and clearly seeing pores with the diameters of 6-8nm which are orderly arranged in the interior.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373328A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院烟台海岸带研究所 | A method of resolution diatom organic matter |
| CN112978738A (en) * | 2021-02-04 | 2021-06-18 | 中国海洋大学 | Method for extracting pure diatom shells from marine unicellular diatoms |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373328A (en) * | 2018-04-13 | 2019-10-25 | 中国科学院烟台海岸带研究所 | A method of resolution diatom organic matter |
| CN112978738A (en) * | 2021-02-04 | 2021-06-18 | 中国海洋大学 | Method for extracting pure diatom shells from marine unicellular diatoms |
Non-Patent Citations (2)
| Title |
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| "Numerical and experimental investigation of light trapping effect of nanostructured diatom frustules";Xiangfan Chen 等;Scientific reports(第5期);第 1-9 页 * |
| 曾贵玉等.《微纳米含能材》.国防工业出版社,2015,(第1版),第110页. * |
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