CN110615459B - Method for preparing spherical vaterite particles by microwave biomineralization - Google Patents
Method for preparing spherical vaterite particles by microwave biomineralization Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a method for preparing spherical vaterite particles by microwave biomineralization, which comprises the following steps: preparing a mixed solution of urea and calcium acetate monohydrate; preparing a urease solution, and adding the urease solution into the mixed solution to obtain a reaction solution; pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, and putting the double-mouth round-bottom flask into a microwave reactor; selecting microwave frequency, and setting microwave reaction temperature, time and stirring magneton rotation rate; carrying out ultrasonic treatment on the reaction product to obtain a suspension, pouring the suspension into a centrifugal tube for centrifugation, and pouring out the supernatant; adding distilled water for ultrasonic cleaning to remove unreacted substances; and drying the collected white particle precipitate to obtain the product. The method accelerates the formation speed of the spherical vaterite particles in the biomineralization process by applying microwaves, controllably adjusts the size of the vaterite particles by changing the concentration of the urease, has high reaction process speed, uses the reagent without pollution, and is environment-friendly.
Description
Technical Field
The invention belongs to the technical field of bionic materials, and particularly relates to a method for preparing spherical vaterite particles by utilizing microwave biomineralization.
Background
Vaterite is one of calcium carbonate, and has various morphologies, such as: spherical, cauliflower-like, hexagonal, etc. Where spherical vaterite is a structure composed of very small primary particles, the size can be adjusted so that the size of the spherical vaterite particles is on the order of microns. The spherical vaterite particle has the characteristics of large specific surface area, high solubility, high dispersibility and the like, and has wide application prospect in the fields of medicine, coating, printing ink, papermaking and the like. The vaterite particles are used as drug carriers and can load drugs such as salicylic acid, and the like, so that the slow release performance of the drugs is improved, and the curative effect of the drugs is better exerted. The ball aragonite particles are added into the coating pigment of the ink-jet paper, the paper has the advantages of high ink absorption speed, high printing quality and the like, and the strength and the ink absorption capacity of the paper can be improved by changing the particle size of the ball aragonite, so that the printing quality of the paper is improved. In the papermaking industry, the vaterite particles can be used as fillers for paper, and improve the brightness, bulk, impermeability and the like of the paper, so that the paper has the advantages of good brightness, writing convenience, uniform coating, firmness, durability, easy drying and the like. There is a need to develop a method for obtaining the spherical vaterite particles rapidly, and the size of the vaterite particles can be controllably adjusted, so as to improve the performance of the vaterite and expand the application range of the vaterite.
In the prior documents or patents, the vaterite particles are mostly prepared by adding additives such as surfactants, which are either polluting to the environment or require a long time to obtain the vaterite by using a biomineralization method. At present, the biomimetic synthesis speed is increased by microwave heating, the biomineralization process is promoted, and a method for preparing spherical vaterite particles by utilizing microwave biomineralization is not reported.
Disclosure of Invention
In view of the problems of the prior art, the invention provides a method for preparing spherical vaterite particles by utilizing microwave biomineralization, aiming at obtaining a method capable of rapidly synthesizing and regulating the size of the spherical vaterite particles.
In order to solve the technical problems, the invention is realized by the following technical scheme: the invention provides a method for preparing spherical vaterite particles by microwave biomineralization, which comprises the following steps:
step S01: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step S02: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.03-0.3 g/L, and the urease activity is about 150 u/mg;
step S03: adding the urease solution into the mixed solution obtained in the step S01 to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9-1: 10;
step S04: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
step S05: selecting microwave frequency, wherein the power range of the microwave reactor is 10-70%;
step S06: setting the reaction temperature within the range of 25-50 ℃, setting the rotation speed of the stirring magnetons within the range of 50-200 revolutions per minute, and setting the reaction time of the microwave reactor within the range of 30-60 minutes;
step S07: carrying out ultrasonic treatment on the reaction product for 2-5 min to obtain a suspension, pouring the suspension into a centrifugal tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
step S08: adding distilled water, carrying out ultrasonic cleaning for 2-5 min, repeating the step S07 for three times, and removing unreacted substances;
step S09: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
Preferably, the frequency range of the microwave reactor in the step S05 is 2400-2500 MHz.
Preferably, under the same conditions, the change of the urease concentration can significantly change the size and distribution of the spherical vaterite particles, and when the urease concentration is about 0.0675g/L, the average size of the spherical vaterite particles is the smallest and the size distribution is more uniform;
preferably, the microwave reaction temperature is about 35 ℃ to significantly increase the reaction rate, and the reaction rate is lower than 25 ℃ or higher than 50 ℃.
From the above, the method for preparing spherical vaterite particles by microwave biomineralization of the invention has at least the following beneficial effects:
1. compared with the prior patents, the method has higher reaction speed for forming the spherical vaterite, can obtain a large amount of spherical vaterite particles within a short time of 30-60 minutes, and the reaction time required for obtaining the spherical vaterite particles by using a biomineralization method in the prior patents is 18-24 hours, such as: patent CN 109295108A.
2. Under the condition that other conditions are not changed, the size of the spherical vaterite particles can be further changed by only changing the concentration of the urease, uniform spherical vaterite particles are obtained, the continuous change of the size of the spherical vaterite particles is realized, and the size of the spherical vaterite particles is firstly reduced and then increased along with the increase of the concentration of the urease, so that the regulation and control of the size of the spherical vaterite particles are realized.
3. During the reaction, the reaction solution is stirred by the stirring magnetons, which facilitates the uniform nucleation of the vaterite, and the nucleation rate can be further controlled by setting the stirring speed, thereby controlling the particle size and distribution of the vaterite.
4. The method has the advantages of wide raw material source, environmental friendliness, simple process and high experimental result repeatability, greatly reduces the reaction time, can further change the size of the spherical vaterite by changing parameters such as reaction temperature, urease concentration, stirring speed and the like, and has good controllability.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments, together with the accompanying drawings.
Drawings
FIG. 1 is an XRD spectrum of the product prepared in example 1 of the present invention;
FIG. 2 is a SEM photograph of the products of examples 1-6 of the present invention, wherein the images (a), (b), (c), (d), (e) and (f) are SEM photographs of the vaterite prepared in examples 1, 2, 3, 4, 5 and 6, respectively;
FIG. 3 shows the particle size and distribution of the products of examples 1 to 6 of the present invention, wherein the graphs (a), (b), (c), (d), (e) and (f) are the vaterite produced in examples 1, 2, 3, 4, 5 and 6, respectively;
FIG. 4 is a graph showing the relationship between the average particle size of vaterite and the concentration of urease in examples 1 to 6 of the present invention.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings, which form a part of this specification, and which illustrate, by way of example, the principles of the invention. In the referenced drawings, the same or similar components in different drawings are denoted by the same reference numerals.
The main experimental raw materials adopted in the embodiment of the invention are as follows: urea is produced by chemical reagent company of national medicine group and has a molecular formula of CH4N2O, purity of 99%. Calcium acetate monohydrate produced by Meclin corporation and having a molecular formula of C4H8CaO5The purity was 98%. Urease was produced by eastern Japan, Inc. and had an activity of 148 u/mg. The distilled water is self-made.
According to the method for preparing the spherical vaterite particles by utilizing microwave biomineralization, the composition components of the product are single-component vaterite within the microwave frequency range of 2400-2500 MHz, the particle morphology is formed by very small primary particles into a spherical shape, and the particle size range is 0.25-18.35 microns. Under the conditions of the same microwave frequency and reaction temperature, the particle size of the vaterite tends to decrease and then increase along with the increase of the urease concentration, and the average particle size value is at least 2.62 μm when the urease concentration is 0.0675 g/L.
Example 1
A method for preparing spherical vaterite particles by microwave biomineralization comprises the following steps:
step 1: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step 2: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.025g/L, and the urease activity is 148 u/mg;
and step 3: adding a urease solution into the mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9;
and 4, step 4: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
and 5: selecting microwave frequency of 2450MHz, wherein the power range of the microwave reactor is 50%;
step 6: setting the reaction temperature to be 35 ℃, setting the rotation rate of the stirring magnetons to be 120 revolutions per minute, and setting the reaction time of the microwave reactor to be 40 minutes;
and 7: carrying out ultrasonic treatment on the reaction product for 3min to obtain a suspension, pouring the suspension into a centrifuge tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
and 8: adding distilled water, ultrasonically cleaning for 3min, repeating the step 7 for three times, and removing unreacted substances;
and step 9: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
FIG. 1 is an XRD pattern of the product prepared in example 1, showing that the predominant species is vaterite; through SEM observation, as shown in FIG. 2(a), the particles are spherical and have good dispersibility; FIG. 3(a) shows that the particle size distribution is narrow, the particle size range is 1.0 to 6.4 μm, and the average particle size is 3.86 μm.
Example 2
A method for preparing spherical vaterite particles by microwave biomineralization comprises the following steps:
step 1: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step 2: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.0675g/L, and the urease activity is 148 u/mg;
and step 3: adding a urease solution into the mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9;
and 4, step 4: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
and 5: selecting microwave frequency of 2450MHz, wherein the power range of the microwave reactor is 50%;
step 6: setting the reaction temperature to be 35 ℃, setting the rotation rate of the stirring magnetons to be 120 revolutions per minute, and setting the reaction time of the microwave reactor to be 40 minutes;
and 7: carrying out ultrasonic treatment on the reaction product for 3min to obtain a suspension, pouring the suspension into a centrifuge tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
and 8: adding distilled water, ultrasonically cleaning for 3min, repeating the step 7 for three times, and removing unreacted substances;
and step 9: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
The product obtained in this example had a composition similar to that of the product of example 1, being single component vaterite; through SEM observation, as shown in FIG. 2(b), the particles are spherical, and have complete spherical shape and good dispersibility; FIG. 3(b) shows that the particle size distribution is narrow, the particle size range is 0.57 to 5.28 μm, and the average particle size is 2.62 μm.
Example 3
A method for preparing spherical vaterite particles by microwave biomineralization comprises the following steps:
step 1: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step 2: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.1g/L, and the urease activity is 148 u/mg;
and step 3: adding a urease solution into the mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9;
and 4, step 4: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
and 5: selecting microwave frequency of 2450MHz, wherein the power range of the microwave reactor is 50%;
step 6: setting the reaction temperature to be 35 ℃, setting the rotation rate of the stirring magnetons to be 120 revolutions per minute, and setting the reaction time of the microwave reactor to be 40 minutes;
and 7: carrying out ultrasonic treatment on the reaction product for 3min to obtain a suspension, pouring the suspension into a centrifuge tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
and 8: adding distilled water, ultrasonically cleaning for 3min, repeating the step 7 for three times, and removing unreacted substances;
and step 9: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
The main material of the product produced in example 3 was vaterite; by SEM observation, as shown in FIG. 2(c), the particles are spherical in shape and more uniform in size; FIG. 3(c) shows that the particle size distribution is narrow, the particle size ranges from 0.74 to 4.0 μm, the particle size ranges from 2.0 to 4.0 μm, and the average particle size is 2.96 μm.
Example 4
A method for preparing spherical vaterite particles by microwave biomineralization comprises the following steps:
step 1: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step 2: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.125g/L, and the urease activity is 148 u/mg;
and step 3: adding a urease solution into the mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9;
and 4, step 4: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
and 5: selecting microwave frequency of 2450MHz, wherein the power range of the microwave reactor is 50%;
step 6: setting the reaction temperature to be 35 ℃, setting the rotation rate of the stirring magnetons to be 120 revolutions per minute, and setting the reaction time of the microwave reactor to be 40 minutes;
and 7: carrying out ultrasonic treatment on the reaction product for 3min to obtain a suspension, pouring the suspension into a centrifuge tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
and 8: adding distilled water, ultrasonically cleaning for 3min, repeating the step 7 for three times, and removing unreacted substances;
and step 9: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
The main component of the product produced in this example 4 was vaterite; by SEM observation, as in fig. 2(d), the particle morphology was nearly spherical; FIG. 3(d) shows the particle size distribution, the particle size range is 0.75 to 14.62 μm, and the average particle size is 3.98. mu.m.
Example 5
A method for preparing spherical vaterite particles by microwave biomineralization comprises the following steps:
step 1: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step 2: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.15g/L, and the urease activity is 148 u/mg;
and step 3: adding a urease solution into the mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9;
and 4, step 4: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
and 5: selecting microwave frequency of 2450MHz, wherein the power range of the microwave reactor is 50%;
step 6: setting the reaction temperature to be 35 ℃, setting the rotation rate of the stirring magnetons to be 120 revolutions per minute, and setting the reaction time of the microwave reactor to be 40 minutes;
and 7: carrying out ultrasonic treatment on the reaction product for 3min to obtain a suspension, pouring the suspension into a centrifuge tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
and 8: adding distilled water, ultrasonically cleaning for 3min, repeating the step 7 for three times, and removing unreacted substances;
and step 9: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
The composition of the product produced in this example 5 was vaterite; by SEM observation, as shown in FIG. 2(e), the particles were spherical in morphology, with a small amount of large particles present; FIG. 3(e) shows the particle size distribution, the particle size ranges from 0.95 to 18.28. mu.m, the particle size ranges from 0.95 to 8.55, and the average particle size is 4.83. mu.m.
Example 6
A method for preparing spherical vaterite particles by microwave biomineralization comprises the following steps:
step 1: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
step 2: preparing a urease solution, and adding urease into distilled water; the concentration range is 0.2g/L, and the urease activity is 148 u/mg;
and step 3: adding a urease solution into the mixed solution obtained in the step (1) to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9;
and 4, step 4: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
and 5: selecting microwave frequency of 2450MHz, wherein the power range of the microwave reactor is 50%;
step 6: setting the reaction temperature to be 35 ℃, setting the rotation rate of the stirring magnetons to be 120 revolutions per minute, and setting the reaction time of the microwave reactor to be 40 minutes;
and 7: carrying out ultrasonic treatment on the reaction product for 3min to obtain a suspension, pouring the suspension into a centrifuge tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
and 8: adding distilled water, ultrasonically cleaning for 3min, repeating the step 7 for three times, and removing unreacted substances;
and step 9: the collected white particle precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
The main component of the product produced in this example 6 was vaterite; by SEM observation, as shown in FIG. 2(f), the particle morphology is spherical; FIG. 3(f) shows the particle size distribution, the particle size range is 4.04 to 18.87 μm, and the average particle size is 8.22 μm.
FIG. 4 is a graph of the urease concentration versus average particle size for the vaterite obtained in examples 1-6 under the same microwave frequency and temperature conditions, with the vaterite particle size tending to decrease and then increase as the urease concentration increases; when the urease concentration is 0.0675g/L, the average particle size value is minimum 2.62 mu m; when the urease concentration is greater than 0.125g/L, the vaterite particle size increases significantly.
The method can quickly obtain the spherical vaterite particles under the microwave condition, and can continuously change the size of the spherical vaterite particles by changing the concentration of the urease.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (4)
1. A method for preparing spherical vaterite particles by microwave biomineralization is characterized by comprising the following steps:
s01: preparing a mixed solution of 0.6mol/L urea and 1mol/L calcium acetate monohydrate;
s02: preparing a urease solution, and adding urease into distilled water, wherein the concentration range is 0.03-0.3 g/L, and the urease activity is 150 u/mg;
s03: adding the urease solution into the mixed solution obtained in the step S01 to obtain a reaction solution, wherein the volume ratio of the urease solution to the mixed solution is 1: 9-1: 10;
s04: pouring the reaction solution into a double-mouth round-bottom flask, putting a stirring magneton into the double-mouth round-bottom flask, putting the double-mouth round-bottom flask into a microwave reactor, connecting a side end interface of the double-mouth round-bottom flask with a thermocouple, connecting a top end interface with a condensing tube, and introducing cooling water into the condensing tube for cooling;
s05: selecting microwave frequency, wherein the power range of the microwave reactor is 10-70%;
s06: setting the reaction temperature within the range of 25-50 ℃, setting the rotation speed of the stirring magnetons within the range of 50-200 revolutions per minute, and setting the reaction time of the microwave reactor within the range of 30-60 minutes;
s07: carrying out ultrasonic treatment on the reaction product for 2-5 min to obtain a suspension, pouring the suspension into a centrifugal tube, centrifuging at 3000rpm for 3min, and pouring out the supernatant;
s08: adding distilled water, carrying out ultrasonic cleaning for 2-5 min, repeating the step S07 for three times, and removing unreacted substances;
s09: the collected white particulate precipitate was dried at 60 ℃ for 24h to give spherical vaterite particles of different sizes.
2. The method for preparing spherical vaterite particles through microwave biomineralization according to claim 1, wherein the frequency range of the microwave reactor in the step S05 is 2400-2500 MHz.
3. The method for preparing spherical vaterite particles through microwave biomineralization as recited in claim 1, wherein in the step S02, the size of the spherical vaterite particles tends to decrease and then increase with the increase of urease concentration, and the average particle size is the smallest when the urease concentration is 0.0675 g/L.
4. The method for preparing spherical vaterite particles through microwave biomineralization according to claim 1, wherein the temperature of the microwave reaction in step S06 is 35 ℃ which can significantly accelerate the mineralization reaction.
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