CN106179408A - A kind of Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material - Google Patents
A kind of Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material Download PDFInfo
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- CN106179408A CN106179408A CN201610552324.5A CN201610552324A CN106179408A CN 106179408 A CN106179408 A CN 106179408A CN 201610552324 A CN201610552324 A CN 201610552324A CN 106179408 A CN106179408 A CN 106179408A
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
A kind of Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material, belongs to technical field of nano material, prepares biomass carbon aeroge with Radix Raphani for raw material；Silver ion in chloride ion in hexadecyltrimethylammonium chloride and silver nitrate generate silver nitride precipitation and be attached to carbon aerogels hole in；Silver chloride in carbon aerogels hole reacts with sodium sulfide, generates the Argentous sulfide. of more indissoluble；Through washing, lyophilization, obtain have load more by force fastness Argentous sulfide. silver load Radix Raphani derive carbon aerogel material.It is applied to process waste water from dyestuff, had both realized the recycling of garbage, and can effectively process again waste water from dyestuff, reach the purpose of the treatment of wastes with processes of wastes against one another.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to the preparation method of carbon aerogel material.
Background technology
Charcoal-aero gel as the nano-porous materials of a kind of lightweight because its to have high porosity, Large ratio surface etc. excellent
Point is quite varied in field application prospects such as catalysis, absorption, electrode material, environmental conservation and energy reserves.Tradition charcoal-aero gel
Preparation method prepared by carbonization phenolic organic aerogel, need a series of behaviour such as high temperature cabonization, supercritical drying process
Make, and phenols, aldehydes have the biggest toxicity, and health and environment are had the biggest danger.
At present, new study hotspot is become with the novel carbon aerogels that biomass are prepared for raw material, due to its surface
There is abundant apparent group, such as C=C, C=O ,-OH, C-O-C etc., modify it, compound, modified etc. is studied further and is provided
Good basis；This material precursor has with low cost, simple and easy to get, advantages of environment protection simultaneously.
Argentous sulfide. is a kind of conventional photocatalyst, and at optics, electricity, sensor, the field such as biomedical has extensively
Application, the synthetic method about Argentous sulfide. nano material substantially has template alive, microemulsion method, organometallic precursor method etc.
Method.Pertinent literature also reports employing new carbon such as Graphene, graphene aerogel etc. and photocatalyst hydridization shape
Become composite, improve the photocatalysis performance of material.The document of Application No. CN201210066145.2 then provides one
As Graphene and the preparation method of Argentous sulfide. nano composite material of ultracapacitor, this Material texture is lighter, reduces cost
It is more beneficial for industrialized production.The document of application number CN201410672172.3 discloses one and quickly prepares Graphene/sulfuration
The preparation method of argentum nano composite material, the method in addition to there is the simple and advantage of low power consuming, mono-layer graphite oxide in solution
The high stability of alkene also ensure that the formation of mono-layer graphite sheet in synthetic, and thus products therefrom has more preferable structure and photoelectricity
Sub-performance.But Graphene pre-treatment is more complicated, building-up process can use poisonous and hazardous Oxidizing and Reducing Agents, the most also needs
To be passed through noble gas in high temperature environments, add production cost and limit its application in actual production.
Summary of the invention
Present invention aim at a kind of environmental protection being provided, preparing simple hydrothermal reaction at low temperature preparation a kind of Argentous sulfide. load
Radix Raphani derives the preparation method of carbon aerogel material.
The present invention comprises the following steps:
1) the block Radix Raphani of peeling is placed at 180 DEG C～200 DEG C and carries out hydro-thermal reaction, obtain biomass carbon base wet gel；
2) biomass carbon base wet gel is soaked in hexadecyltrimethylammonium chloride aqueous solution, then mixes with silver nitrate,
React under the conditions of lucifuge, obtain the carbon aerogels adhering to silver chloride in hole；
3) carbon aerogels adhering to silver chloride in hole is mixed with sodium sulfide, under the conditions of lucifuge, carry out metathesis reaction, take
Obtain system after metathesis reaction；
4) with system after ethanol and distilled water wash metathesis reaction, take solid phase be placed in-15～-18 DEG C of temperature conditionss under freezing,
The most freeze-dried, obtain Argentous sulfide. load Radix Raphani and derive carbon aerogel material.
Biomass derivatives (generally below 200 DEG C) at low temperatures carry out hydrothermal carbonization become prepare sustainable and cheap
The common method of porous carbon materials, briefly, polysaccharide occurs to be dehydrated degradation reaction under hydro-thermal and forms furan intermediate.Then
Defining the carbon ball of micron-scale after experiencing a series of polycondensation and Diels-Alder reaction, size depends primarily on
Hydrothermal temperature and response time.So utilizing multi-functional and multifarious natural precursor can prepare chemical functional characteristic species
The carbon back aerogel material that class is more.
The present invention prepares biomass carbon aeroge with Radix Raphani for raw material in step 1)；In step 2) in cetyl front three
Silver ion in chloride ion in ammonium chloride and silver nitrate generate silver nitride precipitation and be attached to carbon aerogels hole in；
In step 3), the silver chloride in carbon aerogels hole reacts with sodium sulfide, generates the Argentous sulfide. of more indissoluble；Through step 4)
Washing, the chloride ion in removable wet gel and sodium ion, then through lyophilization, obtain and there is the sulfuration loading more by force fastness
Yin Yin load Radix Raphani derives carbon aerogel material.It is applied to process waste water from dyestuff, had both realized the recycling of garbage,
Can effectively process again waste water from dyestuff, reach the purpose of the treatment of wastes with processes of wastes against one another.
Concrete feature:
1, the present invention prepare Argentous sulfide. load Radix Raphani derive during carbon aerogel material without add any surfactant or
Template, does not use organic solvent.
2, the Argentous sulfide. load Radix Raphani that prepared by the present invention derives carbon aerogel material and has abundant raw material, easy and simple to handle, equipment
Simply, the advantage such as operating cost is low.
3, the Argentous sulfide. load Radix Raphani that the present invention prepares derives carbon aerogel material and has good to dyestuffs such as methylene blues
Light degradation effect, when 180min, degradation rate reaches 85%.
Further, in step 1) of the present invention, material hydro-thermal reaction obtained is first with distilled water wash, then with 40
DEG C～the aqueous solution soaking of the ethanol of 45 DEG C wash twice, be then cooled to room temperature, finally clean once with distilled water, obtain raw
Material charcoal base wet gel.Cleaning can remove soluble impurity, soaks and can increase in the aqueous solution of 40 DEG C～the ethanol of 45 DEG C
The framing structure of strong wet gel.
Described step 2) in, the temperature conditions of described reaction is 40 DEG C～45 DEG C.This temperature model is determined through experiment repeatedly
Enclose for optimum reaction condition.
Described step 2) in, described biomass carbon base wet gel is 325～520: 1 with the mixing quality ratio of silver nitrate.Warp
Cross elementary analysis and determine that this mass ratio is wet gel with the quality of silver nitrate than scope, be beneficial to raw material all of, fully
Reaction.
In described step 3), adhering to the carbon aerogels of silver chloride in described hole with the mixing quality ratio of sodium sulfide is 325
～520: 1.Be calculated according to the chemical formula principle of mass conservation, be beneficial to raw material all of, fully react.
In described step 3), the temperature conditions of described metathesis reaction is 40 DEG C～45 DEG C.The bone of wet gel can be strengthened
Shelf structure and preferably allow precipitate be attached in the hole of wet gel.
In described step 4), described cryodesiccated temperature environment is-55 DEG C.
Accompanying drawing explanation
Fig. 1 is the XRD spectra that the Argentous sulfide. load Radix Raphani that the inventive method is made derives carbon aerogel material.
Fig. 2 is the ultraviolet-visible spectrogram that embodiment 1 prepares sample photocatalytic degradation methylene blue.
Fig. 3 is the infared spectrum figure that embodiment 1 prepares sample.
Fig. 4 is the TEM picture that embodiment 1 prepares sample.
Detailed description of the invention
One, preparation method:
Illustrate: each chemical reagent used in the embodiment of the present invention is commercial products.
Embodiment 1
2cm*3cm*4cm size is cut in Radix Raphani peeling, puts it into reactor at 180 DEG C, carry out hydro-thermal reaction 18h.
Material reaction obtained is first with distilled water wash, then the ethanol water washing by soaking two with 40 DEG C～45 DEG C
Secondary, it is then cooled to room temperature, finally cleans once with distilled water, obtain biomass carbon base wet gel.
The hexadecyltrimethylammonium chloride (CTAC) weighing 0.02g is dissolved in the distilled water of 20mL, and ultrasonic vibration makes
It is completely dissolved, and is subsequently adding the biomass carbon base wet gel of 12g and the silver nitrate of 0.025g, at 40 DEG C～the constant temperature of 45 DEG C
Lucifuge reaction 10h in water-bath, obtains the carbon aerogels adhering to silver chloride in precipitate hole after reaction.
In 12g hole, adhere to the sodium sulfide adding 0.025g in the carbon aerogels of silver chloride again, enter under the conditions of lucifuge
Row metathesis reaction, obtains system after metathesis reaction.
After system after metathesis reaction is washed 3 times with ethanol and distillation respectively, topped up with water is put in-15 DEG C of refrigerators freezing
24h, finally puts into freezing 12h in the freezer dryer of-55 DEG C by sample, prepares Argentous sulfide. load Radix Raphani and derives charcoal-aero gel material
Material.
Embodiment 2
2cm*3cm*4cm size is cut in Radix Raphani peeling, puts it into reactor at 200 DEG C, carry out hydro-thermal reaction 18h.
Material reaction obtained is first with distilled water wash, then the ethanol water washing by soaking two with 40 DEG C～45 DEG C
Secondary, it is then cooled to room temperature, finally cleans once with distilled water, obtain biomass carbon base wet gel.
The CTAC weighing 0.02g is dissolved in the distilled water of 20mL, and ultrasonic vibration makes it be completely dissolved, and is subsequently adding 12g
Biomass carbon base wet gel and the silver nitrate of 0.03g, in the water bath with thermostatic control of 40 DEG C～45 DEG C lucifuge reaction 10h, after reaction
Obtain the carbon aerogels adhering to silver chloride in precipitate hole.
In 12g hole, adhere to the sodium sulfide adding 0.03g in the carbon aerogels of silver chloride again, carry out under the conditions of lucifuge
Metathesis reaction, obtains system after metathesis reaction.
After system after metathesis reaction is washed 3 times with ethanol and distillation respectively, topped up with water is put in-18 DEG C of refrigerators freezing
24h, finally puts into freezing 12h in the freezer dryer of-55 DEG C by sample, prepares Argentous sulfide. load Radix Raphani and derives charcoal-aero gel material
Material.
Embodiment 3
2cm*3cm*4cm size is cut in Radix Raphani peeling, puts it into reactor at 180 DEG C, carry out hydro-thermal reaction 20h.
Material reaction obtained is first with distilled water wash, then the ethanol water washing by soaking two with 40 DEG C～45 DEG C
Secondary, it is then cooled to room temperature, finally cleans once with distilled water, obtain biomass carbon base wet gel.
The CTAC weighing 0.03g is dissolved in the distilled water of 20mL, and ultrasonic vibration makes it be completely dissolved, and is subsequently adding 13g
Biomass carbon base wet gel and the silver nitrate of 0.025g, in the water bath with thermostatic control of 40 DEG C～45 DEG C lucifuge reaction 10h, after reaction
Obtain the carbon aerogels adhering to silver chloride in precipitate hole.
In 13g hole, adhere to the sodium sulfide adding 0.025g in the carbon aerogels of silver chloride again, enter under the conditions of lucifuge
Row metathesis reaction, obtains system after metathesis reaction.
After system ethanol after metathesis reaction and distillation are washed 3 times, topped up with water puts into freezing 24h in-16 DEG C of refrigerators,
Finally sample is put into freezing 12h in the freezer dryer of-55 DEG C, obtains Argentous sulfide. load Radix Raphani and derive carbon aerogel material.
Embodiment 4
2cm*3cm*4cm size is cut in Radix Raphani peeling, puts it into reactor at 180 DEG C, carry out hydro-thermal reaction 20h.
Material reaction obtained is first with distilled water wash, then the ethanol water washing by soaking two with 40 DEG C～45 DEG C
Secondary, it is then cooled to room temperature, finally cleans once with distilled water, obtain biomass carbon base wet gel.
The CTAC weighing 0.02g is dissolved in the distilled water of 20mL, and ultrasonic vibration makes it be completely dissolved, and is subsequently adding 13g
Biomass carbon base wet gel and the silver nitrate of 0.035g, in the water bath with thermostatic control of 40 DEG C～45 DEG C lucifuge reaction 10h, after reaction
Obtain the carbon aerogels adhering to silver chloride in precipitate hole.
In 13g hole, adhere to the sodium sulfide adding 0.035g in the carbon aerogels of silver chloride again, enter under the conditions of lucifuge
Row metathesis reaction, obtains system after metathesis reaction.
After system ethanol after metathesis reaction and distillation are washed 3 times, topped up with water puts into freezing 24h in-17 DEG C of refrigerators,
Finally sample is put into freezing 12h in the freezer dryer of-55 DEG C, obtains Argentous sulfide. load Radix Raphani and derive carbon aerogel material.
Embodiment 5
2cm*3cm*4cm size is cut in Radix Raphani peeling, puts it into reactor at 200 DEG C, carry out hydro-thermal reaction 18h.
Material reaction obtained is first with distilled water wash, then the ethanol water washing by soaking two with 40 DEG C～45 DEG C
Secondary, it is then cooled to room temperature, finally cleans once with distilled water, obtain biomass carbon base wet gel.
The CTAC weighing 0.02g is dissolved in the distilled water of 20ml, and ultrasonic vibration makes it be completely dissolved, and is subsequently adding 13g
Biomass carbon base wet gel and the silver nitrate of 0.04g join in above-mentioned solution, keep away in the water bath with thermostatic control of 40 DEG C～45 DEG C
Photoreaction 10h, obtains the carbon aerogels adhering to silver chloride in precipitate hole after reaction.
In 13g hole, adhere to the sodium sulfide adding 0.04g in the carbon aerogels of silver chloride again, carry out under the conditions of lucifuge
Metathesis reaction, obtains system after metathesis reaction.
System ethanol after metathesis reaction and distillation being washed 3 times, rear topped up with water puts into freezing 24h in-18 DEG C of refrigerators,
Finally sample is put into freezing 12h in the freezer dryer of-55 DEG C, obtains Argentous sulfide. load Radix Raphani and derive carbon aerogel material.
Two, characteristic:
The product preparing various embodiments above detects, and testing result is as shown in Figures 1 to 4.
As shown in Figure 1, the strong diffraction maximum of prepared sample at 30 °, 34 °, 38 ° and 55 ° of peak values, all peak values and standard
Spectrogram (JCPDS NO.14-0072) has concordance, shows that the sample of preparation contains Argentous sulfide., and occur at 22 ° is wide special
Levy peak to show in structure containing graphitized carbon, show that sample contains Carbon Materials.Argentous sulfide. load carbon aeroge obtained by explanation
Material is biphase complex
As shown in Figure 2, the photocatalysis performance of sample is fine, the interior degradation rate ＞ 80% to methylene blue simulated wastewater of 180min.
From the figure 3, it may be seen that can be seen that at 1100cm from infrared spectrum-1, 1400cm-1, 1643cm-1, 3132cm-1,
3454cm-1Place has stronger absworption peak consistent with the stretching vibration of Argentous sulfide.；At 890 cm-1The main attribution of absworption peak at place
Plain bending in C-H is vibrated.At 1442 cm-1The peak at place is respectively owing to the stretching vibration of C=O and C=C, at 1120 cm-1The skeletal vibration being mainly due to C-O-C bending vibration or C-C at place, show to only exist in specimen material Argentous sulfide. and
The characteristic peak of two kinds of materials of charcoal-aero gel, shows synthesized to derive carbon aerogel material for Argentous sulfide. load Radix Raphani.
As shown in Figure 4, Argentous sulfide. load Radix Raphani derives the transmission plot of carbon aerogel material, it appeared that in composite
Argentous sulfide. granular size is averagely about 15 nm, and pattern is regular circular granular, and substantial amounts of Argentous sulfide. is carried on biomass carbon
On the surface of base aeroge.
Claims (7)
1. Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material, it is characterised in that comprise the following steps:
1) the block Radix Raphani of peeling is placed at 180 DEG C～200 DEG C and carries out hydro-thermal reaction, obtain biomass carbon base wet gel；
2) biomass carbon base wet gel is soaked in hexadecyltrimethylammonium chloride aqueous solution, then mixes with silver nitrate,
React under the conditions of lucifuge, obtain the carbon aerogels adhering to silver chloride in hole；
3) carbon aerogels adhering to silver chloride in hole is mixed with sodium sulfide, under the conditions of lucifuge, carry out metathesis reaction, take
Obtain system after metathesis reaction；
4) with system after ethanol and distilled water wash metathesis reaction, take solid phase be placed in-15～-18 DEG C of temperature conditionss under freezing,
The most freeze-dried, obtain Argentous sulfide. load Radix Raphani and derive carbon aerogel material.
Preparation method the most according to claim 1, it is characterised in that: in described step 1), the thing that hydro-thermal reaction is obtained
Matter is first with distilled water wash, then washes twice with the aqueous solution soaking of 40 DEG C～the ethanol of 45 DEG C, is then cooled to room temperature, finally
Clean once with distilled water, obtain biomass carbon base wet gel.
Preparation method the most according to claim 1, it is characterised in that: described step 2) in, the temperature conditions of described reaction
It it is 40 DEG C～45 DEG C.
Preparation method the most according to claim 1 and 2, it is characterised in that: described step 2) in, described biomass carbon base is wet
Gel is 325～520: 1 with the mixing quality ratio of silver nitrate.
Preparation method the most according to claim 1, it is characterised in that: in described step 3), described hole adheres to chlorination
The carbon aerogels of silver is 325～520: 1 with the mixing quality ratio of sodium sulfide.
Preparation method the most according to claim 1 or 5, it is characterised in that: in described step 3), described metathesis reaction
Temperature conditions is 40 DEG C～45 DEG C.
Preparation method the most according to claim 1, it is characterised in that: in described step 4), described cryodesiccated temperature
Environment is-55 DEG C.
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Cited By (5)
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| CN106684396A (en) * | 2016-12-21 | 2017-05-17 | 北京化工大学 | Method for preparing bifunctional catalyst from peanut hull |
| CN107983369A (en) * | 2017-11-27 | 2018-05-04 | 江苏大学 | A kind of zinc sulphide load radish derives the preparation method of carbon aerogel material |
| CN112536017A (en) * | 2020-12-22 | 2021-03-23 | 福州大学 | Oil-absorbing white radish-based carbon aerogel and preparation method thereof |
| CN112563042A (en) * | 2020-11-11 | 2021-03-26 | 中国矿业大学 | Biomass carbon aerogel-MnOxPreparation method and application of composite electrode material |
| CN113413870A (en) * | 2021-05-17 | 2021-09-21 | 中国科学院青海盐湖研究所 | Magnesium oxide-metal sulfide-biomass charcoal composite material and preparation method and application thereof |
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| CN113413870A (en) * | 2021-05-17 | 2021-09-21 | 中国科学院青海盐湖研究所 | Magnesium oxide-metal sulfide-biomass charcoal composite material and preparation method and application thereof |
| CN113413870B (en) * | 2021-05-17 | 2022-11-25 | 中国科学院青海盐湖研究所 | Magnesium oxide-metal sulfide-biomass charcoal composite material and preparation method and application thereof |
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Application publication date: 20161207 |