CN107983369A - A kind of zinc sulphide load radish derives the preparation method of carbon aerogel material - Google Patents
A kind of zinc sulphide load radish derives the preparation method of carbon aerogel material Download PDFInfo
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- CN107983369A CN107983369A CN201711205755.5A CN201711205755A CN107983369A CN 107983369 A CN107983369 A CN 107983369A CN 201711205755 A CN201711205755 A CN 201711205755A CN 107983369 A CN107983369 A CN 107983369A
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 46
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 241000220259 Raphanus Species 0.000 title claims abstract description 35
- 235000006140 Raphanus sativus var sativus Nutrition 0.000 title claims abstract description 35
- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 239000002028 Biomass Substances 0.000 claims abstract description 21
- 239000004964 aerogel Substances 0.000 claims abstract description 20
- 239000011240 wet gel Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 14
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 238000006731 degradation reaction Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 238000000859 sublimation Methods 0.000 claims description 2
- 230000008022 sublimation Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 5
- 239000000975 dye Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 7
- 229910052984 zinc sulfide Inorganic materials 0.000 description 7
- 238000004821 distillation Methods 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 238000005698 Diels-Alder reaction Methods 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 briefly Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- 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
-
- B01J35/60—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
The invention belongs to carbon aerogel material preparing technical field, refers in particular to the preparation method that a kind of zinc sulphide load radish derives carbon aerogel material.The present invention prepares biomass carbon aeroge by raw material of radish；Sulphion generation zinc sulphide in zinc ion and thioacetamide in zinc nitrate is precipitated and is attached in the hole of charcoal-aero gel；By washing, the foreign ion in wet gel is can remove, then by freeze-drying, obtain with relatively the zinc sulphide load radish of load fastness derives carbon aerogel material by force.It is applied to processing waste water from dyestuff, has not only realized the recycling of discarded object, but also can effectively handle waste water from dyestuff, achievees the purpose that the treatment of wastes with processes of wastes against one another.
Description
Technical field
The invention belongs to carbon aerogel material preparing technical field, refers in particular to a kind of zinc sulphide load radish and derives charcoal-aero gel
The preparation method of material.
Background technology
Charcoal-aero gel is as a kind of nano-porous materials of lightweight, because it is excellent with high porosity, Large ratio surface etc.
Point is quite varied in field application prospects such as catalysis, absorption, electrode material, environmental protection and energy reserves.Traditional charcoal airsetting
The preparation method of glue is prepared, it is necessary to which high temperature cabonization, supercritical drying process etc. are a series of by carbonizing phenolic organic aerogel
Operation, and phenols, aldehydes have very big toxicity, there is very big danger to body and environment.
At present, new research hotspot is become by new carbon aerogels prepared by raw material of biomass, due to its surface
There are abundant apparent group, such as C=C, C=O ,-OH, C-O-C, the further research such as modify it, are compound, is modified and carrying
Good basis is supplied；The material precursor has of low cost, simple and easy to get, advantages of environment protection at the same time.
Zinc sulphide be it is a kind of have strong electronics constraint ability, stable chemical performance, forbidden band is wide, photoelectric characteristic is excellent, it is nontoxic,
The low semi-conducting material for waiting excellent performance of cost, widely should have in fields such as optics, electricity, sensor, biomedicines
With.Pertinent literature is also reported to be formed using new carbon such as graphene, graphene aerogel etc. with photochemical catalyst hydridization
Composite material, improves the photocatalysis performance of material.The Chinese patent of Application No. CN201611165377.8 provides one kind
The preparation method of graphene and zinc sulfide nano composite material as electrode material, the synthetic method is simple, repeatability
By force, and reduce cost and be more advantageous to industrialized production.The Chinese patent of number of patent application CN201611241695.8 reports one
Kind prepares the preparation method of graphene # zinc sulphide/visible luminescent material of zinc sulfide heterojunction, and the method, which is removed, has simple and low consumption
Outside the advantages of energy, hetero-junctions forms stabilization, is conducive to industrialized production.But graphene pre-treatment is more complicated, building-up process meeting
Poisonous and hazardous Oxidizing and Reducing Agents is used, while also needs to be passed through inert gas in high temperature environments, adds and is produced into
This limits its application in actual production.
The content of the invention
Present invention aims at providing, one kind is environmentally protective, prepares simple hydrothermal reaction at low temperature prepares a kind of zinc sulphide load
Radish derives the preparation method of carbon aerogel material.
The present invention comprises the following steps：
1) the block radish 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 zinc nitrate aqueous solution, then is mixed with thioacetamide, in constant temperature bar
Reacted under part, obtain the charcoal-aero gel for adhering to zinc sulphide in hole；
3) with the system after ethanol and distilled water washing reaction, solid phase is taken to be placed in cold under -15~-18 DEG C of temperature conditionss
Freeze 24h, then it is freeze-dried, obtain zinc sulphide load radish and derive carbon aerogel material.
(generally below 200 DEG C) progress hydrothermal carbonization is sustainable and cheap as preparing at low temperature for biomass derivatives
The common method of porous carbon materials, briefly, polysaccharide occur to be dehydrated degradation reaction formation furan intermediate under hydro-thermal.So
The carbon ball for foring micron-scale by going through after a series of polycondensation and Diels-Alder reactions, size mainly depend on
In hydrothermal temperature and reaction time.So chemical functional spy can be made using multi-functional and multifarious natural precursor
The property more charcoal base aerogel material of species.
The present invention prepares biomass carbon aeroge in step 1) by raw material of radish；Zinc in step 2) in zinc nitrate
Ion is precipitated with the sulphion generation zinc sulphide in thioacetamide and is attached in the hole of charcoal-aero gel；By step
3) washing, can remove the foreign ion in wet gel, then by freeze-drying, obtain with the relatively vulcanization of load fastness by force
Zinc load radish derives carbon aerogel material.It is applied to processing waste water from dyestuff, has not only realized the recycling of discarded object, but also
Waste water from dyestuff can be effectively handled, achievees the purpose that the treatment of wastes with processes of wastes against one another.
Specific feature：
1st, the present invention need not add any surface-active during preparing zinc sulphide load radish and deriving carbon aerogel material
Agent or template, without using organic solvent.
2nd, the zinc sulphide load radish that prepared by the present invention, which derives carbon aerogel material, has abundant raw material, easy to operate, if
It is standby simple, the advantages such as operating cost is low.
3rd, zinc sulphide load radish produced by the present invention, which derives carbon aerogel material, has well the dyestuffs such as methylene blue
Light degradation effect, degradation rate reaches 91% during 180min under visible light illumination.
Further, in step 1) of the present invention, material that hydro-thermal reaction is obtained first to distill water washing, then with
The aqueous solution soaking of ethanol that 40 DEG C~45 DEG C of percent by volume is 80% washes twice, and is subsequently cooled to room temperature, finally with
Distilled water cleans once, obtains biomass carbon base wet gel.
In the step 2), the temperature conditionss of the reaction are 60 DEG C~70 DEG C reaction 6h.
In the step 2), the mixing quality ratio of the biomass carbon base wet gel and zinc nitrate is 20~30: 1.
In the step 2), adhere in described hole zinc nitrate charcoal-aero gel and thioacetamide mass ratio for 90~
100∶1。
In the step 3), the temperature environment of the freeze-drying is -55 DEG C, sublimation drying 12h.
Brief description of the drawings
Fig. 1 is that zinc sulphide made of the method for the present invention loads the XRD spectra that radish derives carbon aerogel material.
Fig. 2 is the light degradation figure 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 pictures that embodiment 1 prepares sample.
Embodiment
First, preparation method：
Explanation：Each chemical reagent used in the embodiment of the present invention is commercial products.
Embodiment 1
3cm*4cm*5cm sizes are cut into radish peeling, reaction kettle is put it into and hydro-thermal reaction 18h is carried out at 180 DEG C.
The material that reaction is obtained is first to distill water washing, then with 40 DEG C~45 DEG C of ethanol water washing by soaking two
It is secondary, room temperature is subsequently cooled to, obtains biomass carbon base wet gel finally cleaning with distilled water once.
Weigh the zinc nitrate (Zn (NO of 0.51g3)2) be dissolved in the distilled water of 20mL, ultrasonic vibration is completely dissolved it,
Then the biomass carbon base wet gel of 12g and the thioacetamide of 0.128g are added, it is anti-in 60 DEG C~70 DEG C of water bath with thermostatic control
6h is answered, sediment is obtained after reaction --- adhere to the charcoal-aero gel of zinc sulphide in hole.
Topped up with water, which is put into -15 DEG C of refrigerators, after system after reaction is washed 3 times with ethanol and distillation respectively freezes
Sample, is finally put into -55 DEG C of freeze drier and freezes 12h by 24h, and zinc sulphide load radish is made and derives charcoal-aero gel material
Material.
Embodiment 2
3cm*4cm*5cm sizes are cut into radish peeling, reaction kettle is put it into and hydro-thermal reaction 20h is carried out at 180 DEG C.
The material that reaction is obtained is first to distill water washing, then with 40 DEG C~45 DEG C of ethanol water washing by soaking two
It is secondary, room temperature is subsequently cooled to, obtains biomass carbon base wet gel finally cleaning with distilled water once.
Weigh the zinc nitrate (Zn (NO of 0.94g3)2) be dissolved in the distilled water of 20mL, ultrasonic vibration is completely dissolved it,
Then the biomass carbon base wet gel of 12g and the thioacetamide of 0.236g are added, it is anti-in 60 DEG C~70 DEG C of water bath with thermostatic control
6h is answered, sediment is obtained after reaction --- adhere to the charcoal-aero gel of zinc sulphide in hole.
Topped up with water, which is put into -15 DEG C of refrigerators, after system after reaction is washed 3 times with ethanol and distillation respectively freezes
Sample, is finally put into -55 DEG C of freeze drier and freezes 12h by 24h, and zinc sulphide load radish is made and derives charcoal-aero gel material
Material.
Example 3
3cm*4cm*5cm sizes are cut into radish peeling, reaction kettle is put it into and hydro-thermal reaction 18h is carried out at 180 DEG C.
The material that reaction is obtained is first to distill water washing, then with 40 DEG C~45 DEG C of ethanol water washing by soaking two
It is secondary, room temperature is subsequently cooled to, obtains biomass carbon base wet gel finally cleaning with distilled water once.
Weigh the zinc nitrate (Zn (NO of 1.42g3)2) be dissolved in the distilled water of 20mL, ultrasonic vibration is completely dissolved it,
Then the biomass carbon base wet gel of 13g and the thioacetamide of 0.358g are added, it is anti-in 60 DEG C~70 DEG C of water bath with thermostatic control
6h is answered, sediment is obtained after reaction --- adhere to the charcoal-aero gel of zinc sulphide in hole.
Topped up with water, which is put into -15 DEG C of refrigerators, after system after reaction is washed 3 times with ethanol and distillation respectively freezes
Sample, is finally put into -55 DEG C of freeze drier and freezes 12h by 24h, and zinc sulphide load radish is made and derives charcoal-aero gel material
Material.
Embodiment 4
3cm*4cm*5cm sizes are cut into radish peeling, reaction kettle is put it into and hydro-thermal reaction 18h is carried out at 180 DEG C.
The material that reaction is obtained is first to distill water washing, then with 40 DEG C~45 DEG C of ethanol water washing by soaking two
It is secondary, room temperature is subsequently cooled to, obtains biomass carbon base wet gel finally cleaning with distilled water once.
Weigh the zinc nitrate (Zn (NO of 3.06g3)2) be dissolved in the distilled water of 20mL, ultrasonic vibration is completely dissolved it,
Then the biomass carbon base wet gel of 12g and the thioacetamide of 0.77g are added, it is anti-in 60 DEG C~70 DEG C of water bath with thermostatic control
5h is answered, sediment is obtained after reaction --- adhere to the charcoal-aero gel of zinc sulphide in hole.
Topped up with water, which is put into -15 DEG C of refrigerators, after system after reaction is washed 3 times with ethanol and distillation respectively freezes
Sample, is finally put into -55 DEG C of freeze drier and freezes 12h by 24h, and zinc sulphide load radish is made and derives charcoal-aero gel material
Material.
Embodiment 5
Weigh the zinc nitrate (Zn (NO of 0.51g3)2) be dissolved in the distilled water of 20mL, ultrasonic vibration is completely dissolved it,
Then the thioacetamide of 0.128g is added, reacts 6h in 60 DEG C~70 DEG C of water bath with thermostatic control, zinc sulphide is obtained after reaction and is sunk
Starch.
Topped up with water, which is put into -15 DEG C of refrigerators, after system after reaction is washed 3 times with ethanol and distillation respectively freezes
Sample, is finally put into -55 DEG C of freeze drier and freezes 12h by 24h, and zinc sulphide monomer material is made.
Embodiment is summarized：The difference of five embodiments exists, the throwing of biomass carbon base aeroge, zinc nitrate, thioacetamide
Material is than different, and the reaction time at the same temperature is different, so as to cause the photocatalysis performance of sample different.
2nd, characteristic：
Product made from various embodiments above is detected, testing result is as shown in Figures 1 to 4.
25wt%ZnS/CA, 40wt%ZnS/CA, 55wt%ZnS/CA, 65wt%ZnS/CA in figure, represent zinc sulphide and exist
Shared quality proportion in biomass carbon base aeroge.
As shown in Figure 1, the strong diffraction maximum of prepared sample goes out on 28.56 °, 47.51 ° and 56.29 ° three positions
Show three characteristic diffraction peaks, corresponded to respectively (111) of ZnS, (220), (311) three diffraction crystal faces, with JCPDC cards
(No1050566) standard spectrogram is consistent, and the sample for showing to prepare contains zinc sulphide, and the quant's sign peak occurred at 22 ° shows
Contain graphitized carbon in structure, show that sample contains carbon material.Illustrate that obtained zinc sulphide load carbon aerogel material is two
Phase compound
As shown in Figure 2, the photocatalysis performance of sample is fine, to the degradation rate ＞ of methylenum careuleum simulated wastewater in 180min
91%.
From the figure 3, it may be seen that in 3450cm-1The absworption peak at place is mainly the stretching vibration of hydroxyl (- OH).1412cm-1With
2902cm-1The absworption peak at place is due to the plain bending vibration of C-H.1620cm-1And 1711cm-1The absworption peak at place is C respectively
The stretching vibration of=O and C=C.1069cm-1It is C-O-C flexural vibrations that the absworption peak at place, which is probably, it is also possible to the skeleton of C-C
Vibration.From infrared spectrum it can be seen that only existing the characteristic peak of two kinds of materials of zinc sulphide and charcoal-aero gel in specimen material, show
Synthesized loads radish derivative carbon aerogel material for zinc sulphide.
As shown in Figure 4, zinc sulphide load radish derives the transmission plot of carbon aerogel material, it can be found that in composite material
Zns particle size is about averagely 120nm, and pattern is regular circular granular, and substantial amounts of zinc sulphide uniform load is in life
On the surface of the carbon-based aeroge of material.
Claims (7)
1. a kind of zinc sulphide load radish derives the preparation method of carbon aerogel material, it is characterised in that：
1) the block radish 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 zinc nitrate aqueous solution, then is mixed with thioacetamide, under constant temperature
Reaction, obtains the charcoal-aero gel for adhering to zinc sulphide in hole；
3) with the system after ethanol and distilled water washing reaction, solid phase is taken to freeze, then it is freeze-dried, obtain zinc sulphide and bear
Carry radish and derive carbon aerogel material.
2. a kind of zinc sulphide load radish as claimed in claim 1 derives the preparation method of carbon aerogel material, its feature exists
In：In the step 1), the material that hydro-thermal reaction is obtained is first to distill water washing, then with 40 DEG C~45 DEG C of percent by volume
Aqueous solution soaking for 80% ethanol washes twice, and is subsequently cooled to room temperature, obtains biology finally cleaning with distilled water once
Matter charcoal base wet gel.
3. a kind of zinc sulphide load radish as claimed in claim 1 derives the preparation method of carbon aerogel material, its feature exists
In：In the step 2), the temperature conditionss of the reaction are 60 DEG C~70 DEG C, reaction time 6h.
4. a kind of zinc sulphide load radish as claimed in claim 1 derives the preparation method of carbon aerogel material, its feature exists
In：In the step 2), the mixing quality ratio of the biomass carbon base wet gel and zinc nitrate is 20~30: 1.
5. a kind of zinc sulphide load radish as claimed in claim 1 derives the preparation method of carbon aerogel material, its feature exists
In：In the step 2), it is 90~100 that the charcoal-aero gel of zinc nitrate and the mass ratio of thioacetamide are adhered in described hole:
1。
6. a kind of zinc sulphide load radish as claimed in claim 1 derives the preparation method of carbon aerogel material, its feature exists
In：In the step 3), the cryogenic temperature is -15~-18 DEG C, cooling time 24h；The temperature environment of the freeze-drying
For -55 DEG C, sublimation drying 12h.
7. a kind of zinc sulphide load radish as claimed in claim 1 derives the preparation method of carbon aerogel material, its feature exists
In：It is 55% that zinc sulphide derives quality proportion shared in carbon aerogel material in zinc sulphide load radish, under visible light illumination
The degradation rate of methylene blue reaches 91% during 180min.
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Cited By (3)
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| CN109225272A (en) * | 2018-10-19 | 2019-01-18 | 郴州高鑫铂业有限公司 | A kind of Pt-ZnS/C catalyst and its preparation method and application |
| CN111072036A (en) * | 2019-12-30 | 2020-04-28 | 石家庄铁道大学 | Preparation method of silicon dioxide aerogel loaded with zinc sulfide |
| CN112536017A (en) * | 2020-12-22 | 2021-03-23 | 福州大学 | Oil-absorbing white radish-based carbon aerogel and preparation method thereof |
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| CN106111175A (en) * | 2016-06-20 | 2016-11-16 | 江苏大学 | A kind of preparation method of tri compound semi-conducting material |
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| CN106111175A (en) * | 2016-06-20 | 2016-11-16 | 江苏大学 | A kind of preparation method of tri compound semi-conducting material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109225272A (en) * | 2018-10-19 | 2019-01-18 | 郴州高鑫铂业有限公司 | A kind of Pt-ZnS/C catalyst and its preparation method and application |
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| CN111072036A (en) * | 2019-12-30 | 2020-04-28 | 石家庄铁道大学 | Preparation method of silicon dioxide aerogel loaded with zinc sulfide |
| CN111072036B (en) * | 2019-12-30 | 2021-07-13 | 石家庄铁道大学 | Preparation method of silicon dioxide aerogel loaded with zinc sulfide |
| CN112536017A (en) * | 2020-12-22 | 2021-03-23 | 福州大学 | Oil-absorbing white radish-based carbon aerogel and preparation method thereof |
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