CN114132928A - Method for preparing silicon carbide nano material by using waste silicon dioxide - Google Patents
Method for preparing silicon carbide nano material by using waste silicon dioxide Download PDFInfo
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- CN114132928A CN114132928A CN202111602265.5A CN202111602265A CN114132928A CN 114132928 A CN114132928 A CN 114132928A CN 202111602265 A CN202111602265 A CN 202111602265A CN 114132928 A CN114132928 A CN 114132928A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 92
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 64
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 55
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 54
- 239000002699 waste material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 229920000642 polymer Polymers 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 6
- 239000002135 nanosheet Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- 239000013049 sediment Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000000634 powder X-ray diffraction Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a method for preparing a silicon carbide nano material by utilizing waste silicon dioxide, which comprises the following steps: (1) mixing waste silicon dioxide, high molecular polymer and metal reducing agent in a closed reactor, and then heating for reaction; (2) and cooling after reaction, washing, filtering and drying the product to obtain the silicon carbide nano material. The method for preparing the silicon carbide nano material by using the waste silicon dioxide adopts a one-step chemical reaction to prepare the silicon carbide nano material, the waste silicon dioxide, the high molecular polymer and the metal reducing agent are placed in a reactor, the heating reaction is carried out, then the cooling is carried out, the product is washed, filtered, separated and dried, and the silicon carbide nano material is obtained, and the yield of the silicon carbide nano material reaches more than 80%; the method for preparing the silicon carbide nano material by utilizing the waste silicon dioxide has the advantages of simple process, cheap raw materials, high product yield and the like.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a method for preparing a silicon carbide nano material by utilizing waste silicon dioxide. The preparation method of the silicon carbide nano material provided by the invention also relates to the technical field of solid waste resource utilization.
Background
Silicon carbide, as a high temperature material, has excellent physical and chemical properties, such as high hardness, high melting point, good chemical stability, high thermal conductivity, and a small thermal expansion coefficient.
At present, the method for preparing silicon carbide mainly comprises the following steps: the method is used for the reduction synthesis method of silica and carbon (J.Mater.Sci.,2004,39, 6057-. The silicon carbide is prepared industrially mainly by carbothermic reduction of silicon dioxide, however, the method for preparing silicon carbide by carbon reduction of silicon dioxide requires higher reaction temperature, the reaction temperature is about 1500 ℃, the reaction conditions are harsh, and the cost is high. Therefore, people are looking for a method for preparing the silicon carbide nano material at a lower temperature by using cheap raw materials and a simple process.
Disclosure of Invention
The invention aims to provide a novel method for preparing a silicon carbide nano material by using waste silicon dioxide, aiming at the problems of higher required reaction temperature, harsh reaction conditions, high preparation cost and the like in the existing silicon carbide preparation process.
The invention is realized by the following technical scheme:
a method for preparing silicon carbide nano material by using waste silicon dioxide is characterized by comprising the following steps:
(1) mixing waste silicon dioxide, high molecular polymer and metal reducing agent in a closed reactor, and then heating for reaction;
(2) and cooling after reaction, washing, filtering and drying the product to obtain the silicon carbide nano material.
Specifically, according to the method for preparing the silicon carbide nano material by using the waste silicon dioxide, the silicon carbide nano material is prepared by adopting a one-step chemical reaction, the waste silicon dioxide, the high-molecular polymer and the metal reducing agent are placed in a reactor, the heating reaction is carried out, then the cooling is carried out, the product is washed, filtered, separated and dried, and the silicon carbide nano material is obtained, wherein the yield of the silicon carbide nano material is over 80 percent.
The raw materials used in the preparation process are wide in source and low in cost, and meanwhile, the waste silicon dioxide is used as the raw material, so that a novel way is developed for resource recycling of the waste silicon dioxide, waste is turned into wealth, and the concept of environment-friendly sustainable development is met.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: mixing the waste silicon dioxide, the high molecular polymer and the metal reducing agent in a reactor, heating to 600-800 ℃ at the speed of 5-10 ℃/min, and carrying out heat preservation reaction for 5-40 hours after the temperature is raised.
The invention provides a novel method for preparing silicon carbide nanosheets by one-step chemical reaction under mild conditions, the reaction temperature required by the method is greatly reduced, the reaction conditions are milder, and the industrial production is easy to realize.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: the mass ratio of the waste silicon dioxide, the high molecular polymer and the metal reducing agent in the step (1) is 1: (0.5-5): (2-10).
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: the waste silicon dioxide in the step (1) is formed by crushing and grinding waste quartz tubes.
The method for preparing the silicon carbide nano material by using the waste silicon dioxide is a silicon carbide nano material preparation process which is mild in reaction condition, wide in raw material source, simple in process and low in cost, wherein the waste silicon dioxide is used as one of raw materials, is derived from a waste quartz tube, and provides a new way for recycling solid wastes of the waste quartz tube, the way not only provides a new treatment way for the solid wastes, but also provides the silicon carbide nano material prepared by the way with high application value; the new treatment mode creates higher added value for the waste quartz tube.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: the high molecular polymer in the step (1) is selected from one or more of polytetrafluoroethylene, polyvinyl chloride and polyethylene.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: the metal reducing agent in the step (1) is magnesium powder.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: the reactor in the step (1) is a stainless steel high-pressure reaction kettle.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: and (3) naturally cooling to room temperature after the reaction in the step (2), washing the product with distilled water, diluted hydrochloric acid and absolute ethyl alcohol in sequence, filtering, washing with hot sodium carbonate solution and diluted hydrochloric acid, and finally drying to obtain the silicon carbide nano material.
Further, the method for preparing the silicon carbide nano material by using the waste silicon dioxide comprises the following steps: the drying in the step (2) is vacuum drying, the drying temperature is 50-60 ℃, and the drying time is 2-5 hours.
The invention provides a new method for preparing silicon carbide nanosheets by one-step chemical reaction under mild conditions, the method has the advantages of simple production equipment required by the preparation process, easiness in realization of industrial production, lower temperature required by the reaction, wide and cheap raw material sources and simplicity in operation, the silicon carbide nanomaterial can be synthesized by one-step chemical reaction, and the yield can reach over 80%.
The invention has the beneficial effects that:
(1) the method for preparing the silicon carbide nano material by using the waste silicon dioxide adopts one-step chemical reaction to prepare the silicon carbide nano material under mild conditions, and has the advantages of simple process, cheap raw materials, high product yield and the like.
(2) The preparation method adopts a closed system, and prepares the silicon carbide nano material in one step through the redox reaction between the metal reducing agent (magnesium powder) and the high molecular polymer and the waste silicon dioxide.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is an X-ray powder diffraction pattern of the silicon carbide nanomaterial prepared in example 1;
FIG. 2 is a field emission scanning photograph of the silicon carbide nanomaterial prepared in example 1;
FIG. 3 is a TEM photograph of the SiC nanomaterial prepared in example 1;
FIG. 4 is an infrared spectrum of a silicon carbide nanomaterial prepared in example 1;
FIG. 5 is an X-ray powder diffraction pattern of the silicon carbide nanomaterial prepared in example 2;
FIG. 6 is a scanning electron microscope photograph of the silicon carbide nanomaterial prepared in example 2;
FIG. 7 is an X-ray powder diffraction pattern of the silicon carbide nanomaterial prepared in example 3;
fig. 8 is a scanning electron microscope photograph of the silicon carbide nanomaterial prepared in example 3.
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. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for preparing a silicon carbide nano material by using waste silicon dioxide comprises the following specific steps:
(1) mixing 0.60g of waste silicon dioxide, 0.50g of polytetrafluoroethylene (high molecular polymer) and 1.20g of magnesium powder in a sealed stainless steel high-pressure reaction kettle, sealing, putting into an electric furnace capable of programmed temperature rise, raising the temperature of the furnace from room temperature to 600 ℃ within 80 minutes, and maintaining the reaction at 600 ℃ for 10 hours after the temperature rise is finished; products in the stainless steel high-pressure reaction kettle comprise black sediments and residual gas;
(2) and naturally cooling to room temperature after reaction, collecting black sediments adhered to the inner wall of the reaction kettle, washing the product for multiple times by using distilled water, dilute hydrochloric acid and absolute ethyl alcohol, filtering and separating to obtain a sample, repeatedly washing the obtained sample for multiple times by using a hot sodium carbonate solution and dilute hydrochloric acid, and drying the washed sample in a vacuum drying oven at 50 ℃ for 4 hours to obtain the silicon carbide nano material.
The reaction mechanism of example 1 above is as follows:
SiO2+2Mg→2MgO+Si*；2Mg+1/n[C2F4]n＝2C+2MgF2；
Si*+C*→SiC
phase analysis was performed on the silicon carbide nanomaterial prepared in example 1 using a japanese Rigaku D/max- γ a X-ray powder diffraction (XRD) instrument; cu
Graphite monochromator, tube pressure and current respectively40kV and 40mA, and the scanning speed is 10.0 degrees per minute; the analysis result is shown in fig. 1, and fig. 1 is an X-ray diffraction spectrum of the product prepared in example 1; as can be seen from fig. 1, all diffraction peaks at 10 to 80 ° in the X-ray diffraction spectrum, in which the diffraction intensity is high and the peak shape is sharp, can be labeled as cubic phase and hexagonal phase silicon carbide SiC, and no other impurity peak is present. The morphology, particle size, etc. of the product of example 1 were observed using a field emission scanning electron microscope (FESEM, JEOL JSM-6300F), the observation results of which are shown in fig. 2; as can be seen from the field emission scanning electron microscope photograph of the product of FIG. 2, the silicon carbide sample obtained by the method of the present invention is composed of nanosheets, the size of the silicon carbide nanosheets being 200nm, and the thickness being about 20 nm. From the transmission electron micrograph (fig. 3) of the product, it can also be seen that the silicon carbide sample obtained by the method of the present invention is composed of silicon carbide nanosheets. From the infrared spectrum of the product, as can be seen in FIG. 4, the product silicon carbide nanosheets are at about 821cm-1There is a strong absorption peak nearby, this peak is attributed to the transverse photon vibrational mode of the Si — C bond, which indicates that the product produced is silicon carbide, and the strong and sharp peak shape indicates that the sample has a higher crystallinity.
Example 2
A method for preparing a silicon carbide nano material by using waste silicon dioxide comprises the following specific steps:
(1) mixing 0.60g of waste silicon dioxide, 0.50g of polytetrafluoroethylene (high molecular polymer) and 1.20g of magnesium powder in a sealed stainless steel high-pressure reaction kettle, sealing, putting into an electric furnace capable of programmed heating, heating the furnace temperature from room temperature to 800 ℃ within 80 minutes, and maintaining the reaction at 800 ℃ for 5 hours after the heating is finished; products in the stainless steel high-pressure reaction kettle comprise black sediments and residual gas;
(2) and naturally cooling to room temperature after reaction, collecting black sediments adhered to the inner wall of the reaction kettle, washing the product for multiple times by using distilled water, dilute hydrochloric acid and absolute ethyl alcohol, filtering and separating to obtain a sample, repeatedly washing the obtained sample for multiple times by using a hot sodium carbonate solution and dilute hydrochloric acid, and drying the washed sample in a vacuum drying oven at 60 ℃ for 3 hours to obtain the silicon carbide nano material.
Fig. 5 is an X-ray diffraction pattern of the product prepared in example 2, and as can be seen from fig. 5, all diffraction peaks at 10 to 80 ° in 2 θ in the X-ray diffraction pattern can be labeled as cubic phase and hexagonal phase silicon carbide, and no other impurity peaks appear, confirming that the sample prepared in example 2 is a silicon carbide material. The particle size and the like of the product obtained in example 2 are observed by using a field emission scanning electron microscope, and the result is shown in fig. 6, and as can be seen from a field emission scanning electron microscope photo shown in fig. 6, the silicon carbide nanosheet obtained by the method disclosed by the invention is composed of nanoparticles, the average thickness of the silicon carbide nanosheet is 20nm, and the size of the silicon carbide nanosheet is non-uniform. The above analysis confirmed that silicon carbide nanoplates can be prepared by the method of the present invention, and the yield of silicon carbide was calculated to be 80% from the mass of the product silicon carbide and the mass of silicon dioxide.
Example 3
A method for preparing a silicon carbide nano material by using waste silicon dioxide comprises the following specific steps:
(1) mixing 0.60g of waste silicon dioxide, 0.80g of polyvinyl chloride (high molecular polymer) and 1.20g of magnesium powder in a sealed stainless steel high-pressure reaction kettle, sealing, putting into an electric furnace capable of programmed heating, heating the furnace temperature from room temperature to 700 ℃ within 80 minutes, and maintaining the reaction at 700 ℃ for 40 hours after the heating is finished; products in the stainless steel high-pressure reaction kettle comprise black sediments and residual gas;
(2) and naturally cooling to room temperature after reaction, collecting black sediments adhered to the inner wall of the reaction kettle, washing the product for multiple times by using distilled water, dilute hydrochloric acid and absolute ethyl alcohol, filtering and separating to obtain a sample, and then drying the obtained sample in a vacuum drying oven at 55 ℃ for 5 hours to obtain the silicon carbide nano material.
FIG. 7 is an X-ray diffraction pattern of the product prepared in example 3, in which all diffraction peaks can be scaled to cubic phase of silicon carbide
No other impurity peaks were present. Using field emission scanning electron microscopy (FESEM, JEOL JSM-6)300F) The morphology, particle size, etc. of the product were observed, and as shown in fig. 8, it can be seen from the field emission scanning photograph of the product of fig. 8 that the silicon carbide sample obtained by the method of the present invention was composed of a sheet shape. The above analysis confirmed that silicon carbide nanomaterial could be prepared by this method, with a yield of 70% silicon carbide based on the mass of the product silicon carbide and the mass of the silica.
Examples 4-9 are substantially the same as example 1, except as noted in the process data of table 1.
Table 1 shows the process parameters of the silicon carbide nanomaterials of examples 4 to 9
The invention provides a new method for preparing silicon carbide nano material by one-step chemical reaction under mild conditions, which has the advantages of low temperature required by the reaction, wide and cheap raw material source, simple operation, easy realization of industrial production and high yield of silicon carbide product.
The above-mentioned preferred embodiments of the present invention are provided for illustration only and not for the purpose of limiting the invention. Obvious variations or modifications of the present invention are within the scope of the present invention.
Claims (9)
1. A method for preparing silicon carbide nano material by using waste silicon dioxide is characterized by comprising the following steps:
(1) mixing waste silicon dioxide, high molecular polymer and metal reducing agent in a closed reactor, and then heating for reaction;
(2) and cooling after reaction, washing, filtering and drying the product to obtain the silicon carbide nano material.
2. The method as claimed in claim 1, wherein the step (1) comprises mixing the waste silica, the high molecular polymer and the metal reducing agent in a reactor, heating to 800 ℃ at a rate of 5-10 ℃/min, and maintaining the temperature for 5-40 hours after the heating.
3. The method for preparing the silicon carbide nano material by using the waste silicon dioxide as claimed in claim 1, wherein the mass ratio of the waste silicon dioxide, the high molecular polymer and the metal reducing agent in step (1) is 1: (0.5-5): (2-10).
4. The method for preparing silicon carbide nano-materials by using the waste silicon dioxide as claimed in claim 1, wherein the waste silicon dioxide in the step (1) is formed by crushing and grinding waste quartz tubes.
5. The method for preparing silicon carbide nano-materials by using waste silicon dioxide as claimed in claim 1, wherein the high molecular polymer in step (1) is one or more selected from polytetrafluoroethylene, polyvinyl chloride and polyethylene.
6. The method for preparing silicon carbide nano-materials by using waste silicon dioxide as claimed in claim 1, wherein the metal reducing agent in step (1) is magnesium powder.
7. The method for preparing silicon carbide nano-materials by using waste silicon dioxide as claimed in claim 1, wherein the reactor in the step (1) is a stainless steel autoclave.
8. The method for preparing the silicon carbide nano material by using the waste silicon dioxide as claimed in claim 1, wherein the silicon carbide nano material is obtained by cooling to room temperature after the reaction in the step (2), washing the product with distilled water, diluted hydrochloric acid and absolute ethyl alcohol in sequence, filtering, washing with hot sodium carbonate solution and diluted hydrochloric acid, and finally drying.
9. The method for preparing silicon carbide nanomaterial by using waste silicon dioxide according to claim 1, wherein the drying in the step (2) is vacuum drying, the drying temperature is 50-60 ℃, and the drying time is 2-5 hours.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5340417A (en) * | 1989-01-11 | 1994-08-23 | The Dow Chemical Company | Process for preparing silicon carbide by carbothermal reduction |
| WO2000030974A1 (en) * | 1998-11-20 | 2000-06-02 | Clemson University | Process for recycling spent pot liner |
| CN101386409A (en) * | 2008-10-16 | 2009-03-18 | 昆明理工大学 | Method for preparing silicon carbide nano line |
| CN101525134A (en) * | 2009-04-02 | 2009-09-09 | 山东大学 | Method for preparing cubic silicon carbide ultrafine powder by using waste plastic at low temperature |
| CN101774813A (en) * | 2010-01-20 | 2010-07-14 | 中国科学院山西煤炭化学研究所 | Method for preparing small-sized silicon carbide or silicon nitride nano particles from waste plastics |
| CN107416837A (en) * | 2017-05-09 | 2017-12-01 | 武汉科技大学 | A kind of method that porous nano carborundum is prepared using silicate glass as raw material |
| CN111453733A (en) * | 2020-06-10 | 2020-07-28 | 中南民族大学 | Nano β -silicon carbide and preparation method thereof |
| CN112093801A (en) * | 2020-05-11 | 2020-12-18 | 武汉科技大学 | Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof |
-
2021
- 2021-12-24 CN CN202111602265.5A patent/CN114132928A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5340417A (en) * | 1989-01-11 | 1994-08-23 | The Dow Chemical Company | Process for preparing silicon carbide by carbothermal reduction |
| WO2000030974A1 (en) * | 1998-11-20 | 2000-06-02 | Clemson University | Process for recycling spent pot liner |
| CN101386409A (en) * | 2008-10-16 | 2009-03-18 | 昆明理工大学 | Method for preparing silicon carbide nano line |
| CN101525134A (en) * | 2009-04-02 | 2009-09-09 | 山东大学 | Method for preparing cubic silicon carbide ultrafine powder by using waste plastic at low temperature |
| CN101774813A (en) * | 2010-01-20 | 2010-07-14 | 中国科学院山西煤炭化学研究所 | Method for preparing small-sized silicon carbide or silicon nitride nano particles from waste plastics |
| CN107416837A (en) * | 2017-05-09 | 2017-12-01 | 武汉科技大学 | A kind of method that porous nano carborundum is prepared using silicate glass as raw material |
| CN112093801A (en) * | 2020-05-11 | 2020-12-18 | 武汉科技大学 | Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof |
| CN111453733A (en) * | 2020-06-10 | 2020-07-28 | 中南民族大学 | Nano β -silicon carbide and preparation method thereof |
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