CN113860310A - Method for extracting nanoscale silicon carbide from superfine silicon carbide tailings - Google Patents
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Abstract
The invention discloses a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, which comprises the following steps of adding silicon carbide superfine powder tailings into a reactor with a water-alcohol ratio of 1: 2-3: 1, fully and uniformly mixing, standing, naturally settling, and centrifuging the supernatant remained after natural settling, wherein the centrifugal speed is controlled at 5000-. The method can better extract the nanoscale silicon carbide from the superfine silicon carbide tailings, has high extraction efficiency, reduces the cost of enterprises, and increases the income of enterprises producing silicon carbide by the method.
Description
Technical Field
The invention relates to a production process of silicon carbide, in particular to a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings.
Background
The silicon carbide material has excellent physical and chemical properties such as higher elastic modulus, good heat conductivity coefficient, difficult corrosion, low specific gravity compared with metal materials, good heat conductivity and the like, so that the silicon carbide material is widely regarded by people, the silicon carbide is actively researched and explored, the silicon carbide is more finely and richly recognized, and the related application fields of the silicon carbide are further widened, such as the fields of abrasive tools, semiconductor materials, electric automobiles, nuclear fuel particle coatings, electrocatalysis, astronomy and the like.
The traditional preparation method of silicon carbide is to mix coke and quartz sand, utilize petroleum coke raw materials contained in the coke and rich silicon dioxide raw materials in the quartz sand, then add NaCl and saw dust to fully stir and mix, place the mixed and stirred mixture in a high temperature furnace, raise the temperature in the furnace to about 2000 ℃, fire, finally through various different physical and chemical processes, extract and finally obtain silicon carbide micropowder. But the silicon carbide micro powder obtained finally has a large amount of fine-grained material residues after classification and purification, which causes lost sales, and the tailings have a large amount of nano-grade silicon carbide, which has great advantages for various fields to change the nano-grade silicon carbide into more excellent products.
Disclosure of Invention
The invention aims to solve the technical problem of providing the method for extracting the nanoscale silicon carbide in the superfine silicon carbide tailings, which is reasonable in design and good in extraction and separation effects, aiming at the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting nano-scale silicon carbide from superfine silicon carbide tailings is characterized in that the method comprises the following steps of adding silicon carbide superfine powder tailings into a mixture with a water-alcohol ratio of 1: 2-3: 1, fully and uniformly mixing, standing, naturally settling, and centrifuging the supernatant remained after natural settling, wherein the centrifugal speed is controlled at 5000-.
The technical problem to be solved by the invention can also be realized by the following technical scheme that the method comprises the following specific steps,
1) taking water and alcohol in a ratio of 1: 2-3: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding the silicon carbide ultrafine powder tailing into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 2-7 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 1 to 3 days;
4) and after the standing is finished, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 8000-.
The technical problem to be solved by the invention can also be realized by the following technical scheme that in the step 4), the centrifugal rotating speed is 12000 r, and the centrifugal time is 10 minutes.
The technical problem to be solved by the invention can also be realized by the following technical scheme, in the step 1), the water-alcohol ratio of the pure glycol solution is controlled to be 1: 1 or 2: 1.
compared with the prior art, the invention adopts the following steps that the water-alcohol ratio is 2: 1 or a water-alcohol ratio of 1: the solution 1 is used for fully and uniformly mixing the superfine silicon carbide tailings, the supernatant is subjected to centrifugation after natural sedimentation, the centrifugal rotating speed is controlled to 8000-14000 revolutions and the centrifugation lasts for 5-12 minutes, and the obtained nano silicon carbide has good extraction effect, high separation efficiency and uniform and good granularity.
Drawings
FIG. 1 is a graph of particle size analysis of silicon carbide tailings from a certain enterprise;
FIG. 2 is a graph showing a particle size distribution of purified and separated silicon carbide, measured by centrifuging a pure water solution for 5 minutes at different centrifugal speeds;
FIG. 3 is a graph showing a particle size distribution of purified and separated silicon carbide, measured by centrifuging a pure aqueous solution for 10 minutes at different centrifugal speeds;
FIG. 4 is a line graph of the distribution of the pure aqueous solution at 5 minutes centrifugation D50;
FIG. 5 is a line graph of the distribution of the pure aqueous solution at 10 minutes centrifugation D50;
FIG. 6 is a graph showing the particle size distribution of purified and separated silicon carbide, measured by centrifuging a pure ethylene glycol solution for 5 minutes at different centrifugation speeds;
FIG. 7 is a graph showing the particle size distribution of purified and separated silicon carbide, measured by centrifuging a pure ethylene glycol solution for 10 minutes at different centrifugation speeds;
FIG. 8 is a line graph of the distribution of pure ethylene glycol solution at 5 min centrifugation D50;
FIG. 9 is a line graph of the distribution of pure ethylene glycol solution at 10 min centrifugation D50;
FIG. 10 shows a water-alcohol ratio of 1: 1, centrifuging the solution for 5 minutes, and measuring the particle size distribution diagram of the purified and separated silicon carbide at different centrifugal rotating speeds;
FIG. 11 shows a water-alcohol ratio of 1: 1, centrifuging the solution for 10 minutes, and measuring the particle size distribution diagram of the purified and separated silicon carbide at different centrifugal rotating speeds;
fig. 12 shows the ratio of water to alcohol of 1: 1 solution centrifuge D50 distribution line graph for 5 minutes;
fig. 13 shows the ratio of water to alcohol 1: 1 solution centrifuge D50 distribution line graph for 10 minutes;
FIG. 14 water to alcohol ratio 1: 2, centrifuging the solution for 5 minutes, and measuring the particle size distribution diagram of the purified and separated silicon carbide at different centrifugal rotating speeds;
FIG. 15 water to alcohol ratio 1: 2, centrifuging the solution for 10 minutes, and measuring the particle size distribution diagram of the purified and separated silicon carbide at different centrifugal rotating speeds;
FIG. 16 shows the ratio of water to alcohol is 2: 1, centrifuging the solution for 5 minutes, and measuring the particle size distribution diagram of the purified and separated silicon carbide at different centrifugal rotating speeds;
FIG. 17 shows the ratio of water to alcohol is 2: 1, centrifuging the solution for 10 minutes, and measuring the particle size distribution diagram of the purified and separated silicon carbide at different centrifugal rotating speeds;
fig. 18 shows the water to alcohol ratio 2: 1 solution centrifuge D50 distribution line graph for 5 minutes;
fig. 19 shows the water to alcohol ratio 2: 1 solution centrifuge D50 distribution line graph for 10 minutes;
FIG. 20 is a graph showing the particle size distribution of silicon carbide separated at 8000 revolutions for 5 minutes for various solution systems;
FIG. 21 is a graph showing the particle size distribution of silicon carbide separated at 8000 revolutions for 10 minutes for various solution systems;
FIG. 22 is a graph showing the particle size distribution of silicon carbide separated from a solution system at 10000 rpm for 5 minutes;
FIG. 23 is a graph of particle size distribution of silicon carbide separated at 10000 rpm for 10 minutes for various solution systems;
FIG. 24 is a graph of particle size distribution of silicon carbide separated at 12000 rpm for 5 minutes for various solution systems;
FIG. 25 is a graph of particle size distribution of silicon carbide separated at 12000 rpm for 10 minutes for various solution systems;
FIG. 26 is a graph showing particle size distribution of silicon carbide separated at 14000 rpm for 5 minutes for various solution systems;
FIG. 27 is a graph showing the particle size distribution of silicon carbide separated at 14000 rpm for 10 minutes for various solution systems;
fig. 28 shows the ratio of water to alcohol 1: 1, separating and extracting a 5-minute centrifugal particle size distribution diagram from a solution system;
fig. 29 shows the ratio of water to alcohol 1: 1 particle size distribution by 10 min centrifugation of the solution system.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
A method for extracting nano-scale silicon carbide from superfine silicon carbide tailings comprises the following steps of adding silicon carbide superfine powder tailings into a mixture of water and alcohol in a ratio of 1: 2-3: 1, fully and uniformly mixing, standing, naturally settling, and centrifuging the supernatant remained after natural settling, wherein the centrifugal speed is controlled at 5000-.
Example 1, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) taking water and alcohol in a ratio of 1: 2 in a beaker,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 8000 revolutions, the centrifugation time is 5 minutes, and filtering after centrifugation to obtain the nano-silicon carbide.
Embodiment 2, a method for extracting nano-scale silicon carbide from superfine silicon carbide tailings, which comprises the following steps,
1) the ratio of water to alcohol is 3: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 16000 r, the centrifugation time is 12 min, and filtering after centrifugation to obtain the nano-scale silicon carbide.
Example 3, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) taking water and alcohol in a ratio of 1: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 12000 r, the centrifugation time is 10 minutes, and filtering after centrifugation to obtain the nano-scale silicon carbide.
Example 3, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) taking water and alcohol in a ratio of 1: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 10000 r, the centrifugation time is 10 minutes, and filtering after centrifugation to obtain the nano-scale silicon carbide.
Example 4, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) the ratio of water to alcohol is 2: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 12000 r, the centrifugation time is 8 minutes, and filtering after centrifugation to obtain the nano-scale silicon carbide.
Example 5, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) the ratio of water to alcohol is 2: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 10000 r, the centrifugation time is 10 minutes, and filtering after centrifugation to obtain the nano-scale silicon carbide.
Example 6, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) taking water and alcohol in a ratio of 1: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 8000 revolutions, the centrifugation time is 12 minutes, and filtering after centrifugation to obtain the nano-scale silicon carbide.
Example 7, a method for extracting nanoscale silicon carbide from superfine silicon carbide tailings, comprising the following steps,
1) the ratio of water to alcohol is 2: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding 50g of silicon carbide ultrafine powder tailings into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 5 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 days;
4) and after standing, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 14000 r revolutions, the centrifugation time is 8 minutes, and filtering after centrifugation to obtain the nano-scale silicon carbide.
The invention adopts natural sedimentation, and the principle is that carborundum with different granularities is subjected to different buoyancy and gravity in solution and finally distributed in different layers, large particles are precipitated at the bottom of a container, nano-scale small particles are distributed at the upper layer in the solution to form turbid liquid, the liquid is extracted and centrifuged to finally obtain carborundum with nano-scale particles, the centrifugation is controlled by time and rotating speed, and finally the nano carborundum obtained by detection is measured by a laser granularity tester.
The following experiments were conducted on the effect of extracting nano-silicon carbide from the tailings of silicon carbide ultrafine powder with solutions of different systems, different centrifugal speeds and different centrifugal times, and the specific conditions were as follows:
1.1 test devices and drugs
1.1.1 test apparatus
1000ml beaker, 800ml beaker, 50ml beaker, 500ml graduated cylinder, glass cup, pipette, centrifuge tube, timer, sampling spoon, sampling paper, crucible tongs. Other instruments are shown in Table 1-1.
TABLE 1-1 Instrument models and Place of origin
1.1.2 test drugs
6000-mesh silicon carbide waste tailings, deionized water and ethylene glycol in a certain enterprise.
1.2 test procedure
a. 50g of silicon carbide waste tailings of a certain enterprise were sampled and placed on dry and clean medical paper.
b. 1000ml of deionized water was taken in a 1000ml beaker.
c. The removed material was added to a beaker, stirred with a glass rod and placed in an ultrasonic instrument for 5 minutes.
d. And after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 2 d.
e. After the rest is finished, the liquid on the middle and upper layers is taken out by a pipette and is placed in a beaker for later use.
f. Repeating the operation, wherein the water-alcohol ratio of the solution is 1: 1. 1: 2. 2: 1 and pure ethylene glycol solution.
g. And taking out the obtained solution, adding the solution into a centrifugal tube, centrifuging, and changing the centrifuging time and the centrifuging rotating speed to obtain different nano silicon carbide.
h. And placing the obtained nano silicon carbide into a laser particle size tester for detection and identification.
i. Inductive summary data for analysis
2 nano silicon carbide separation and extraction research
2.1 analysis of purification data for different solution systems
2.1.1 analysis of the starting Material
The method comprises the following steps that (1) laser particle size analysis testing is carried out on tailings left by silicon carbide produced by a certain enterprise; FIG. 1 shows experimental results of particle size measurements obtained from silicon carbide tailings from a certain enterprise. According to the result chart, the particle size distribution of 6000-mesh (2.5 microns) silicon carbide tailings produced by the enterprise is wide, and D5 is 0.837 nm; d90 is 4.206um, which contains a plurality of nano-scale silicon carbide particles, the particles exist in tailings, the substances are greatly wasted, and the nano-scale silicon carbide is a very meaningful substance for us. From the particle size distribution diagram, the average particle size of the silicon carbide tailings is 2.506 micrometers, and the proportion of nano-scale silicon carbide in the tailings is relatively low, so that a reasonable control mode should be adopted during the experiment to prevent the experiment from failing due to operation errors.
2.1.2 analysis of extraction centrifugation of pure aqueous solution
Fig. 2 and 3 are particle size distribution diagrams of solutions in a pure water system of deionized water, which are measured by centrifugation for 5 minutes and 10 minutes, and centrifugation speeds of 8000 revolutions, 10000 revolutions, 12000 revolutions and 14000 revolutions, respectively, after natural sedimentation for two days. The distribution of D50 is shown by the line chart of fig. 4 and fig. 5, and finally, the comprehensive analysis shows that the solution with pure water as the system can be finally purified and separated to obtain nano-scale silicon carbide particles. However, in contrast, the higher the centrifugal speed, the wider and wider the particle size obtained, and the longer the time, the more particles are separated, and further, the extraction and separation by pure water can meet the requirements of people only by selecting proper centrifugal speed. Most importantly, pure water is found to have poor controllability, so that the solution cannot be used for settlement during extraction of enterprises.
2.1.3 analysis of extraction centrifugation of pure ethylene glycol solution
Fig. 6 and 7 are graphs showing particle size distributions of pure ethylene glycol solutions measured by centrifugation for 5 minutes and 10 minutes, and centrifugation speeds of 8000, 10000, 12000 and 14000 revolutions, respectively, after two days of natural sedimentation. The particles of D50 from which they were isolated are shown in fig. 8 and 9. Through comprehensive analysis of the four graphs, the solution system separates the nanometer silicon carbide particles in the enterprise tailings, and the particles separated and extracted in 5 minutes are relatively and uniformly distributed, but the separation and extraction pair in 10 minutes is relatively wider in difference and wider in distribution range compared with the separation and extraction pair in 5 minutes. Therefore, the nano-scale silicon carbide particles with relatively concentrated particle size distribution can be obtained by centrifugally selecting a pure ethylene glycol solution system for 5 minutes.
2.1.4 Water to alcohol ratio 1: 1 analysis of extraction centrifugation of solutions
Fig. 10 and 11 show the ratio of water to alcohol of 1: 1 is a comparison graph of the particle size distribution graph of the solution of the system, measured finally by centrifugation for 5 minutes and 10 minutes, and at centrifugation speeds of 8000, 10000, 12000 and 14000 revolutions, respectively, after two days of natural settling. The system solution of the D50 particles separated from the system solution is shown in FIGS. 12 and 13. Comprehensive analysis of the data shows that the ratio of water to alcohol is 1: 1, the nano-scale silicon carbide obtained after the solution system is finally centrifuged for 10 minutes is more uniformly and intensively distributed, more obtained particles have no great relation with the rotating speed, and nano-scale particles extracted by centrifugation for 5 minutes are relatively widely distributed. The final option was to centrifuge for 10 minutes after precipitation for further extraction.
2.1.5 Water to alcohol ratio 1: 2 analysis of extraction centrifugation of solutions
Fig. 14 and 15 show the ratio of water to alcohol of 1: and 2 is a comparison graph of particle size distribution graphs of the solution of the system, which are finally measured by centrifugation for 5 minutes and 10 minutes and centrifugation rotating speeds of 8000 revolutions, 10000 revolutions, 12000 revolutions and 14000 revolutions respectively after natural sedimentation for two days. As can be seen from the comprehensive comparison, the water-alcohol ratio is 1: the solution of 2 system is difficult to separate the nanometer silicon carbide particles. The solution protocol is not recommended.
2.1.6 Water to alcohol ratio of 2: 1 analysis of extraction centrifugation of solutions
FIGS. 3-16 and FIGS. 3-17 are the ratio of water to alcohol of 1: and 2 is a comparison graph of particle size distribution graphs of the solution of the system, which are finally measured by centrifugation for 5 minutes and 10 minutes and centrifugation rotating speeds of 8000 revolutions, 10000 revolutions, 12000 revolutions and 14000 revolutions respectively after natural sedimentation for two days. The distribution of the D50 particles separated from the system solution is shown in fig. 18 and 19. Comprehensive analysis shows that the solution is very suitable for extracting nano-scale silicon carbide, the extraction range is concentrated, the distribution is narrow, and the waste of particles is little. D90 is also a particle that is all on the nanometer scale, not beyond the nanometer scale. The peak line measured by the laser particle size tester is also high and narrow. Is particularly suitable for extracting and separating nano silicon carbide and can meet the requirements of people. But relatively speaking, the faster the rotating speed, the longer the time, which is very helpful for extraction.
2.2 analysis of the data extracted by the separation at centrifugal speed
2.2.1 comprehensive comparison at 8000 rpm of centrifugal speed
Referring to fig. 20 and 21, in summary, the results obtained by comprehensive analysis, we can find that the separation results are best obtained under the condition of the same centrifugal rotating speed, that water is greater than pure ethylene glycol and the ratio of water to alcohol is greater than 1: 1 is greater than the ratio of water to alcohol of 2: 1 is greater than the ratio of water to alcohol of 1: 2, in comparison, the longer the rotational speed time, the better the efficiency of the resulting nanosized silicon carbide.
2.2.2 comprehensive comparison at a centrifugal speed of 10000 revolutions
Referring to fig. 22 and 23, the centrifugal efficiency is higher than 8000 rpm, and the purification and fractionation efficiency is effectively improved for different solutions. The water-alcohol ratio is 1: the solution 2 has a less obvious effect on the graded purification, and basically cannot separate nano-grade silicon carbide nano-particles, and the comprehensive analysis may cause the stress of the particles to be greatly changed due to a solution system, so that the requirements of the graded purification cannot be met, and for time, the longer the solution is reflected, the better the distribution of the purified and graded particles is.
2.1.1 comprehensive comparison at a centrifugal speed of 12000 revolutions
Referring to fig. 24 and 25, after the experiment of 12000 rpm, the particle size distribution is more concentrated, and the obtained particle size is finer, and the minimum particle size can reach about 100 nm, as shown by the laser particle size tester, under the condition of 12000 rpm, the efficiency of extraction and classification is lower than the previous efficiency of 8000 and 10000 rpm, and as shown by analysis, the nano silicon carbide particles extracted by drying finally are lost due to centrifugation under the condition of aqueous solution. Water is more soluble than other solutions and therefore will lose its solubility with water after centrifugation.
2.2.4 comprehensive comparison at 14000 revolutions of centrifugal speed
Referring to fig. 26 and 27, in summary, in the experiment of 14000 rpm, it can be further found that when the water-alcohol ratio is 1: 1, the finally obtained nano silicon carbide is most stable. The particle size results measured by the laser particle size analyzer are compared with each other, and finally, the higher the rotating speed is, the more the silicon carbide is separated, and the silicon carbide extracted by the last group of pure deionized water solution contains nano-sized and micron-sized silicon carbide. For analysis reasons, the solution taken out for operational reasons caused the aspiration of the underlying precipitated silicon carbide particles, resulting in the solution not finally belonging to the solution after standing.
3.3 analysis of data extracted by centrifugation time on separation
Referring to fig. 28 and 29, a better optimized system water-alcohol ratio of 1: 1, the same solution, the same rotating speed and different centrifugation time are shown in the research and analysis of the separation and extraction test of the system solution, and finally, after the determination of a laser particle size tester, the obtained nano-silicon carbide has different relevant quality, the centrifugation efficiency of 10 minutes is completely different even in the centrifugation of 5 minutes, the remarkable special width of the distribution of the separated and extracted silicon carbide can be found in the centrifugation of 5 minutes, the distribution of different particle sizes is also nonuniform, and the number of nano-particles is obviously less than that in the centrifugation of 10 minutes. Further analysis revealed that the particle size in the supernatant was not completely separated and extracted. Compared with the final particle size distribution measured after 10 minutes of centrifugation, the final particle size distribution is wider, and the volume of each particle size is obviously increased, which indicates that the longer the centrifugation time is, the more abundant the finally obtained nano silicon carbide is, and the amount of the silicon carbide with 100 nanometers which is difficult to separate is also obviously increased.
In summary, five different solution systems, namely pure deionized water, pure ethylene glycol solution and a water-alcohol ratio of 1: 1, the ratio of water to alcohol is 1: 2, the ratio of water to alcohol is 2: 1; then, carrying out centrifugation at four centrifugation rotating speeds (8000 revolutions, 10000 revolutions, 12000 revolutions and 14000 revolutions) and two centrifugation times (5 minutes and 10 minutes) to finally obtain nanometer-grade silicon carbide particles in the high-purity superfine tailings; and finally, detecting the extracted nano silicon carbide particles by a laser particle size tester. Through comprehensive analysis of test results, the following conclusions can be obtained:
(1) the water-alcohol ratio is 2: 1 or a water-alcohol ratio of 1: 1, the rotation speed of the centrifugation is 12000 revolutions, and the centrifugation for 10 minutes is an optimized scheme. The nano-scale silicon carbide separated by the two schemes has better particle size distribution, and the water-alcohol ratio is 2: 1 had a D10 of 0.251; d90 was 0.613 and D50 was 0.441. The water-alcohol ratio is 1: 1 had a D10 of 0.313; d90 was 0.689 and D50 was 0.483. The nano-scale silicon carbide extracted and separated by the two solutions is more concentrated and has more particles.
(2) The pure glycol solution can extract nanometer silicon carbide particles on a certain basis, but slightly smaller micron silicon carbide particles can also be extracted, and finally, the extracted and separated silicon carbide particles comprise the nanometer silicon carbide particles and fine micron silicon carbide particles and cannot completely meet the requirements required by people.
(3) The solution of pure water can separate out the nanometer-scale silicon carbide, but if a little external factors exist, the nanometer-scale silicon carbide cannot be completely separated and purified, and the raw material waste is caused.
(4) The water-alcohol ratio is 1: the solution 2 cannot distinguish the nanometer silicon carbide from the solution, and the silicon carbide is still mixed and distributed in the solution, which does not meet the requirements required by the experimental design.
Finally, comparison concludes that the water-alcohol ratio is 2: 1 or a water-alcohol ratio of 1: 1, the rotation speed of the centrifugation is 12000 revolutions, and the centrifugation for 10 minutes is an optimized separation and extraction scheme.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A method for extracting nano-scale silicon carbide from superfine silicon carbide tailings is characterized in that the method comprises the following steps of adding silicon carbide superfine powder tailings into a mixture with a water-alcohol ratio of 1: 2-3: 1, fully and uniformly mixing, standing, naturally settling, and centrifuging the supernatant remained after natural settling, wherein the centrifugal speed is controlled at 5000-.
2. The method for extracting the nano-scale silicon carbide in the superfine silicon carbide tail material as claimed in claim 1, which comprises the following steps,
1) taking water and alcohol in a ratio of 1: 2-3: 1 in a beaker of 1000ml of pure ethylene glycol solution,
2) adding the silicon carbide ultrafine powder tailing into a beaker filled with pure ethylene glycol solution, stirring by using a glass rod, and putting into an ultrasonic instrument for ultrasonic treatment for 2-7 minutes;
3) after the ultrasonic treatment is finished, taking out the beaker, placing the beaker in a clean and dry place, and standing the beaker to naturally settle for 1 to 3 days;
4) and after the standing is finished, taking out the supernatant by using a pipette, placing the supernatant into a centrifugal tube for centrifugation, wherein the centrifugation speed is 8000-.
3. The method for extracting nano-scale silicon carbide from superfine silicon carbide tailings as claimed in claim 2, wherein in the step 4), the centrifugal rotation speed is 12000 r, and the centrifugal time is 10 min.
4. The method for extracting nano-scale silicon carbide from superfine silicon carbide tailings according to claim 2 or 3, wherein in the step 1), the water-alcohol ratio of the pure ethylene glycol solution is controlled to be 1: 1 or 2: 1.
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