CN108314050A - A kind of preparation method of the nanometer silicon carbide particle of efficient absorption organic dyestuff - Google Patents
A kind of preparation method of the nanometer silicon carbide particle of efficient absorption organic dyestuff Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0251—Compounds of Si, Ge, Sn, Pb
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The present invention relates to a kind of preparation methods of the nanometer silicon carbide particle of efficient absorption organic dyestuff, belong to adsorbent technology of preparing and water environment field of purification.This method using sucrose etc. be carbon source, nitrate is catalyst, sodium metasilicate etc. for silicon source, carbon silicon binary xerogel is prepared for by sol-gal process, then by it under argon gas or nitrogen atmosphere protection in 1,000 1400oC carries out carbothermic reduction reaction, and reaction obtains primary product after being cooled to room temperature, and primary product is first 500 800oIt is calcined in C air, removes unreacted carbon, then impregnated in acid and remove within 24 72 hours other impurities object etc., washing, drying obtain nanometer silicon carbide particle.It is added in dye wastewater solution using nanometer silicon carbide particle as sorbing material, is used as the adsorbent of dye wastewater treatment.The easy to operate, equipment requirement of the present invention is simple, economical and effective, and the nanometer silicon carbide specific grain surface product of preparation is relatively high, be it is a kind of can be recycled, the sorbing material of efficient dye wastewater treatment, and there is excellent absorption property.
Description
Technical field
The present invention relates to a kind of preparation method of nanometer silicon carbide particle, related in particular to it is a kind of have efficiently,
The preparation method of recyclable organic dye adsorbent namely belongs to adsorbent technology of preparing and water environment field of purification.
Background technology
Organic synthetic dye is in industries such as plastics, weaving, leather, cosmetics, papermaking, printing, dyestuff manufacture, food processings
In be widely used, millions of ton of waste water from dyestuff is directly discharged.Since dyestuff is mostly benzene series, naphthalene system, anthraquinone, benzene
Amine and diphenyl amine compound, and majority has the characteristics that property is stable, color is high, eco-toxicity is big, thus intractability
Larger, effect on environment is big, is one of typical bio-refractory, difficult organic industrial sewage.Therefore, waste water from dyestuff is straight
Run in and put and will constitute a serious threat to ecological environment and human health, these toxic dyes are removed or decomposed from waste water and are had become
One main environmental problem.Up to the present, the processing method for being applied to dye dye waste water is relatively more, mainly there is flocculation sediment
Method, hyperfiltration, absorption method, chemical coagulation, photocatalytic degradation, membrane separation process and oxidizing process etc..In these processing methods,
Absorption method has many advantages, such as that easy to operate, at low cost, environmental-friendly, good separating effect, adsorption capacity are big, it has also become very efficiently
Dye waste water treatment method, obtained wide model application.The development and utilization of adsorbent is the key factor of adsorption treatment, is commonly used
Adsorbent include activated carbon, organobentonite, clay, molecular sieve etc., but due to the use of the originals such as of high cost, treatment effeciency is low
The application of cause, adsorption treatment is subject to certain restrictions, thus it is at absorption to seek adsorbent economic, efficient, can be recycled
The key of reason.
The features such as nanometer silicon carbide particle has grain size small, and specific surface is big, thus show excellent mechanical property, photoelectricity
Characteristic, chemical stability and biocompatibility etc., in fields such as optical device, electronics, adsorbent, catalytic carrier and composite materials
The application prospect shown.Therefore, the preparation of nanometer silicon carbide particle causes the extensive concern of people, many methods by with
In the synthesis and preparation of nanometer silicon carbide particle.The common method for preparing nanometer silicon carbide particle has carbothermic method, chemistry
Vapour deposition process, Polycarbosilane pyrolysismethod, hydrothermal synthesis method, laser irradiation etc..Such as Chinese patent（Notification number：CN
104310402 A）Disclose a kind of method preparing nanometer silicon carbide particle.This method respectively with agriculture waste biomass, just
Silester and cobalt nitrate are carbon source, silicon source and catalyst, by sol-gel method and carbothermic reduction reaction 1300oUnder C
Constant temperature 7 hours is prepared for the nanometer silicon carbide particle being evenly distributed.For another example, Chinese patent（Notification number：101774813A）It is open
A kind of method preparing small-sized silicon carbide nano particle.This method is first by the waste plastic after cleaning in 600-1000oC
It is carbonized under argon gas atmosphere, then carbonized product is mixed with the Silica abrasive of load ferric nitrate, by mixture in argon gas
In 1100-1400 under atmosphereoC carries out carbothermic reduction reaction 3-20 hours, is prepared for small-sized silicon carbide nano particle.In addition,
Document（J. Nanopart. Res., 2004, 6, 63-70）Using CO2Laser pyrolysis processes are from C2H2And SiH4Mixed flow reactor
In be prepared for a diameter of 10 nanometers of SiC particulate.Using silica flour and graphite as raw material, using simple, low-cost high energy mechanical
Spheroidal graphite method is prepared for nanometer silicon carbide particle（J. Nanosci. Nanotechnol., 2010, 10, 1951-1955）.Though
Right nanometer silicon carbide particle is produced by many methods, but is still rarely had by application in waste water from dyestuff improvement as sorbing material
Report.
Invention content
The object of the present invention is to provide it is a kind of it is easily operated, equipment requirement is simple, cost-effective prepares high-specific surface area
The method of nanometer silicon carbide particle.
The invention is characterized in that using sol-gel method and low temperature carbothermic reduction reaction, it is prepared for nanometer silicon carbide particle,
The material be it is a kind of can be recycled, the sorbing material of efficient dye wastewater treatment, and have excellent absorption property.
The present invention is achieved by means of the following methods：（1）Weigh the nitric acid of the carbon source and 0.1-0.5 parts by weight of 1 parts by weight
The acid of the solvent and 0.1-0.2 parts by weight of 2-4 parts by weight is added in beaker in salt, and stirring is allowed to dissolve, and forms solution A.
（2）The silicon source of 2-4 parts by weight is weighed, under stirring conditions, the deionized water of 4-6 parts by weight is added, is formed molten
Liquid B.
（3）Solution B is slowly added drop-wise in solution A, silicon source hydrolyzes 12-72 hours at room temperature, forms carbon silicon binary colloidal sol.
（4）The curing agent of 0.1-0.3 parts by weight is added, accelerates colloidal sol solidification, carbon silicon binary gel is formed, then in 80-
120 oIt is 6-12 hours dry under the conditions of C, obtain carbon silicon binary xerogel.
（5）The carbon silicon binary xerogel that will be obtained, in certain atmosphere, with 2-10oThe heating rate of C/min is heated to
1000-1400 oC, constant temperature 2-10 hours, is cooled to room temperature.
（6）Product is first in 500-800oIt aoxidizes 2-5 hours in C air, then is impregnated 24-72 hours in acid, washing is done
It is dry to get to porous silicon carbide nano silicon particles.
（7）0.1 parts by weight silicon-carbide particle is weighed, is added in dye wastewater solution, it is molten to survey its at regular intervals
The absorbance of liquid, it is to be adsorbed reach balance after, calculate the adsorption efficiency and capacity of sample.
Carbon source as described above is phenolic resin, sucrose, glucose etc..
Nitrate as described above is ferric nitrate, cobalt nitrate, nickel nitrate, lanthanum nitrate, copper nitrate or zinc nitrate etc..
Acid as described above is nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid etc..
Silicon source as described above is sodium metasilicate, potassium silicate, methyl silicon sodium alcoholate, methyl silanol potassium etc..
Curing agent as described above is hexamethylenetetramine.
Atmosphere as described above is nitrogen, argon gas etc..
Dyestuff as described above is methylene blue, methyl orange, rhodamine B, benzene series, naphthalene system, anthraquinone, aniline and diphenyl amine
Compound etc..
The present invention is to have prepared high-ratio surface silicon carbide nano particle, the ratio of sample with a kind of easy-to-use method
Surface area is in 20-300 m2Between/g, grain size is between 50-100 nanometers.
Specific implementation mode
Embodiment 1
（1）2.5 grams of sucrose and 1.5 grams of ferric nitrates are weighed in beaker, 20 milliliters of water stirrings are added and are allowed to dissolve, 6.5 millis are added
6 mol/L hydrochloric acid solutions are risen, stirring obtains solution A.
（2）5.0 grams of sodium metasilicate are weighed in another beaker, 20 ml deionized waters are added, stirring is allowed to dissolve, and is formed molten
Liquid B.
（3）Solution B is slowly added drop-wise in solution A, silicon source hydrolyzes 24 hours at room temperature, forms carbon Ludox.
（4）2 milliliters of hexamethylenetetramine solution are added, accelerates colloidal sol solidification, carbon silicon binary gel is formed, then 110oIt is 12 hours dry under the conditions of C, obtain carbon silicon binary xerogel.
（5）By binary xerogel obtained, in argon gas stream（200 ml/min）Under, with 10oThe heating rate of C/min adds
Heat is to 1150oC, constant temperature 6 hours, is cooled to room temperature.
（6）Product is first 700oAoxidize 2 hours in C air, then impregnated 72 hours in hydrochloric acid, washed, it is dry to get
To SiC nano particles.
（7）Weigh 30 milligrams of silicon-carbide particles, be added in methylene blue simulated wastewater solution, every 20 minutes, sampling, from
The heart, surveys the absorbance of its supernatant liquor, it is to be adsorbed reach balance after, calculate the adsorption efficiency and capacity of sample.
Embodiment 2
（1）2.5 grams of sucrose and 1.5 grams of nickel nitrates are weighed in beaker, 20 milliliters of water stirrings are added and are allowed to dissolve, 6.5 millis are added
6 mol/L salpeter solutions are risen, stirring obtains solution A.
（2）5.0 grams of sodium metasilicate are weighed in another beaker, 20 ml deionized waters are added, stirring is allowed to dissolve, and is formed molten
Liquid B.
（3）Solution B is slowly added drop-wise in solution A, silicon source hydrolyzes 24 hours at room temperature, forms carbon Ludox.
（4）2 milliliters of hexamethylenetetramine solution are added, accelerates colloidal sol solidification, carbon silicon binary gel is formed, then 110oIt is 12 hours dry under the conditions of C, obtain carbon silicon binary xerogel.
（5）By binary xerogel obtained, in argon gas stream（100 ml/min）Under, with 10oThe heating rate of C/min adds
Heat is to 1100oC, constant temperature 8 hours, is cooled to room temperature.
（6）Product is first 700oAoxidize 2 hours in C air, then impregnated 72 hours in hydrochloric acid, washed, it is dry to get
To SiC nano particles.
（7）Weigh 40 milligrams of silicon-carbide particles, be added in rhodamine B simulated wastewater solution, every 20 minutes, sampling, from
The heart, surveys the absorbance of its supernatant liquor, it is to be adsorbed reach balance after, calculate the adsorption efficiency and capacity of sample.
Embodiment 3
（1）2.5 grams of phenolic resin and 1.5 grams of nickel nitrates are weighed in beaker, 20 milliliters of water stirrings are added and are allowed to dissolve, are added
6.5 milliliter of 6 mol/L hydrochloric acid solution, stirring, obtains solution A.
（2）5.0 grams of potassium silicates are weighed in another beaker, 20 ml deionized waters are added, stirring is allowed to dissolve, and is formed molten
Liquid B.
（3）Solution B is slowly added drop-wise in solution A, silicon source hydrolyzes 24 hours at room temperature, forms carbon Ludox.
（4）2 milliliters of hexamethylenetetramine solution are added, accelerates colloidal sol solidification, carbon silicon binary gel is formed, then 100oIt is 12 hours dry under the conditions of C, obtain carbon silicon binary xerogel.
（5）By binary xerogel obtained, in nitrogen stream（200 ml/min）Under, with 10oThe heating rate of C/min adds
Heat is to 1000oC, constant temperature 6 hours, is cooled to room temperature.
（6）Product is first 700oAoxidize 2 hours in C air, then impregnated 72 hours in hydrochloric acid, washed, it is dry to get
To SiC nano particles.
（7）Weigh 30 milligrams of silicon-carbide particles, be added in methyl orange simulated wastewater solution, every 20 minutes, sampling, from
The heart, surveys the absorbance of its supernatant liquor, it is to be adsorbed reach balance after, calculate the adsorption efficiency and capacity of sample.
Embodiment 4
（1）2.5 grams of glucose and 1.5 grams of cobalt nitrates are weighed in beaker, 20 milliliters of water stirrings are added and are allowed to dissolve, are added 6.5
6 mol/L salpeter solutions of milliliter, stirring obtain solution A.
（2）5.0 grams of methyl silicon sodium alcoholates are weighed in another beaker, 20 ml deionized waters are added, stirring is allowed to dissolve, shape
At solution B.
（3）Solution B is slowly added drop-wise in solution A, silicon source hydrolyzes 24 hours at room temperature, forms carbon Ludox.
（4）2 milliliters of hexamethylenetetramine solution are added, accelerates colloidal sol solidification, carbon silicon binary gel is formed, then 110oIt is 12 hours dry under the conditions of C, obtain carbon silicon binary xerogel.
（5）By binary xerogel obtained, in argon gas stream（200 ml/min）Under, with 10oThe heating rate of C/min adds
Heat is to 1300oC, constant temperature 4 hours, is cooled to room temperature.
（6）Product is first 700oAoxidize 2 hours in C air, then impregnated 72 hours in hydrochloric acid, washed, it is dry to get
To SiC nano particles.
（7）Weigh 40 milligrams of silicon-carbide particles, be added in methylene blue simulated wastewater solution, every 20 minutes, sampling, from
The heart, surveys the absorbance of its supernatant liquor, it is to be adsorbed reach balance after, calculate the adsorption efficiency and capacity of sample.
Claims (13)
1. the invention is characterized in that using sol-gel technique, the carbon silicon binary that is prepared as raw material using nitrate, carbon source and silicon source
Xerogel, progress carbothermic reduction reaction is prepared for nanometer silicon carbide particle in reaction gas（In the preparation process of colloidal sol, due to
The generation of salt, hence it is evident that reduce the temperature of carbothermic reduction reaction）, unreacted carbon and institute are removed by air oxidation and pickling
The impurity such as the metal oxide contained, it is washing, dry to get to nanometer silicon carbide particle, using nanometer silicon carbide particle as inhaling
Enclosure material is in the processing of waste water from dyestuff.
2. the carbon silicon binary xerogel in claim 1 is dissolved in solvent by carbon source and nitrate, silicon source, room is then added
Colloidal sol is formed through acid-catalyzed hydrolysis under temperature, colloidal sol curing agent hexamethylenetetramine is added, obtains carbon silicon binary gel, gel is again
It is dried under certain condition, obtains xerogel.
3. the carbon source in claim 1 and 2 can be sucrose, glucose, phenolic resin etc..
4. the silicon source in claim 1 and 2 can be sodium metasilicate, potassium silicate, methyl silicon sodium alcoholate, methyl silanol potassium etc..
5. the nitrate in claim 1 and 2 can be the nitrate such as nickel nitrate, ferric nitrate, cobalt nitrate, magnesium nitrate, it acts as
Auxiliary agent.
6. the acid in claim 1 and 2 can be hydrochloric acid, nitric acid, sulfuric acid etc., it acts as silicon source hydrolysts.
7. the reaction gas in claim 1 is nitrogen, argon gas, the size of air-flow is 50-200 ml/min.
8. the temperature of carbothermic reduction reaction is 1000 in claim 1oC-1400 oC, constant temperature time are 2-10 hours, heating
Rate is 2-10oC/min。
9. the temperature of air oxidation is 600 in claim 1oC-800 oC, oxidization time are 2-5 hours.
10. dry temperature is 80 in claim 2oC-110 oC, drying time are 4-12 hours.
11. dyestuff is methylene blue, methyl orange, rhodamine B, benzene series, naphthalene system, anthraquinone, aniline and benzidine in claim 1
Class compound etc..
12. carbon source in claim 2, nitrate, solvent, silicon source, the weight ratio of acid and hexamethylenetetramine are：1：0.1-
0.2：2-4：4-6：0.1-0.3：0.1-0.3.
13. the specific surface area of the nanometer silicon carbide particle obtained in claim 1 is in 20-300 m2Between/g, grain size is in 50-
Between 100 nanometers.
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Cited By (10)
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| CN109052402A (en) * | 2018-08-16 | 2018-12-21 | 陕西科技大学 | A kind of method of the continuous preparation pure phase carbonization iron nano-particle of green |
| CN109133310A (en) * | 2018-07-26 | 2019-01-04 | 锐达工业科技（南京）有限公司 | A kind of novel solid dephosphorization agent and preparation method thereof |
| CN109437913A (en) * | 2018-12-27 | 2019-03-08 | 沈阳大学 | A kind of method that low temperature is synthetically prepared Silicon Carbide Powder |
| CN110252403A (en) * | 2019-06-18 | 2019-09-20 | 重庆化工职业学院 | A kind of composite photocatalyst material and its preparation method and application |
| CN110518224A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of preparation method of lithium ion battery carbon silicon anode material |
| CN111036255A (en) * | 2019-12-11 | 2020-04-21 | 河北大学 | Preparation method and application of reed-based SiC/C photocatalytic hydrogen production catalytic material |
| CN113447495A (en) * | 2021-06-29 | 2021-09-28 | 国网黑龙江省电力有限公司电力科学研究院 | High-temperature metal surface flaw detection method |
| CN113666375A (en) * | 2021-09-06 | 2021-11-19 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
| CN114682280A (en) * | 2022-04-11 | 2022-07-01 | 南方科技大学 | Nickel monoatomic catalyst and its preparation method and use |
| CN115259160A (en) * | 2022-07-20 | 2022-11-01 | 哈尔滨工业大学 | Preparation method of SiC nano powder |
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Cited By (14)
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| CN109133310A (en) * | 2018-07-26 | 2019-01-04 | 锐达工业科技（南京）有限公司 | A kind of novel solid dephosphorization agent and preparation method thereof |
| CN109052402A (en) * | 2018-08-16 | 2018-12-21 | 陕西科技大学 | A kind of method of the continuous preparation pure phase carbonization iron nano-particle of green |
| CN109437913B (en) * | 2018-12-27 | 2021-08-24 | 沈阳大学 | Method for preparing silicon carbide ceramic powder by low-temperature synthesis |
| CN109437913A (en) * | 2018-12-27 | 2019-03-08 | 沈阳大学 | A kind of method that low temperature is synthetically prepared Silicon Carbide Powder |
| CN110252403A (en) * | 2019-06-18 | 2019-09-20 | 重庆化工职业学院 | A kind of composite photocatalyst material and its preparation method and application |
| CN110518224A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of preparation method of lithium ion battery carbon silicon anode material |
| CN111036255A (en) * | 2019-12-11 | 2020-04-21 | 河北大学 | Preparation method and application of reed-based SiC/C photocatalytic hydrogen production catalytic material |
| CN113447495A (en) * | 2021-06-29 | 2021-09-28 | 国网黑龙江省电力有限公司电力科学研究院 | High-temperature metal surface flaw detection method |
| CN113666375A (en) * | 2021-09-06 | 2021-11-19 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
| CN113666375B (en) * | 2021-09-06 | 2023-10-27 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
| CN114682280A (en) * | 2022-04-11 | 2022-07-01 | 南方科技大学 | Nickel monoatomic catalyst and its preparation method and use |
| CN114682280B (en) * | 2022-04-11 | 2024-01-12 | 南方科技大学 | Nickel monoatomic catalyst and preparation method and application thereof |
| CN115259160A (en) * | 2022-07-20 | 2022-11-01 | 哈尔滨工业大学 | Preparation method of SiC nano powder |
| CN115259160B (en) * | 2022-07-20 | 2024-05-03 | 哈尔滨工业大学 | Preparation method of SiC nano powder |
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Application publication date: 20180724 |