CN109225189A - Be carbonized peanut shell load nano-titanium dioxide material and preparation method thereof - Google Patents
Be carbonized peanut shell load nano-titanium dioxide material and preparation method thereof Download PDFInfo
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- CN109225189A CN109225189A CN201811218361.8A CN201811218361A CN109225189A CN 109225189 A CN109225189 A CN 109225189A CN 201811218361 A CN201811218361 A CN 201811218361A CN 109225189 A CN109225189 A CN 109225189A
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- 235000017060 Arachis glabrata Nutrition 0.000 title claims abstract description 117
- 235000010777 Arachis hypogaea Nutrition 0.000 title claims abstract description 117
- 235000018262 Arachis monticola Nutrition 0.000 title claims abstract description 117
- 235000020232 peanut Nutrition 0.000 title claims abstract description 117
- 239000000463 material Substances 0.000 title claims abstract description 90
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 241001553178 Arachis glabrata Species 0.000 title claims abstract 25
- 238000003763 carbonization Methods 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 22
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 238000010521 absorption reaction Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 9
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000000975 dye Substances 0.000 abstract description 5
- 239000012265 solid product Substances 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract 1
- 244000105624 Arachis hypogaea Species 0.000 description 92
- 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 description 50
- 229960000907 methylthioninium chloride Drugs 0.000 description 50
- 239000007788 liquid Substances 0.000 description 16
- 239000003463 adsorbent Substances 0.000 description 11
- 238000002835 absorbance Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 6
- 239000012086 standard solution Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000000643 oven drying Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000002028 Biomass Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002154 agricultural waste Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002551 biofuel Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000003911 water pollution 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to field of environmental improvement, it is related to a kind of carbonization peanut shell load nano-titanium dioxide material and preparation method thereof.Milled peanut shell is mixed with titanium sulfate aqueous solution first and potassium hydroxide solution is added after standing adjusts the pH value of mixed liquor to alkalinity, heating reaction is carried out after the mixed liquor for adjusting pH value is packed into hydrothermal reaction kettle sealing again, solid product is collected by filtration after the reaction was completed, washing, it is dry, obtain carbonization peanut shell load nano-titanium dioxide material.Synchronously completing for the load of the carbonization and nano-titanium dioxide of peanut shell in carbonization peanut shell, while the preferable microstructure for keeping carbonization peanut shell may be implemented in this method, improves the combination of nano-titanium dioxide and the peanut shell that is carbonized.Prepared carbonization peanut shell load nano-titanium dioxide material has both good absorption and photocatalysis performance, can efficiently complete the degradation to the organic dyestuff in water, which is also able to maintain good performance during reuse.
Description
Technical field
The present invention relates to a kind of carbonization peanut shell load nano-titanium dioxide materials and preparation method thereof, and in particular to utilizes
Natural peanut shell is the carbonization that raw material realizes peanut shell by one step of hydro-thermal reaction and nano-titanium dioxide in carbonization peanut shell
In load, to prepare carbonization peanut shell load nano-titanium dioxide material, prepared carbonization peanut shell loads nanometer two
Titania meterial can be used for the removal of Organic substance in water.
Background technique
With modern industry, agricultural development, various approach enter water body chemical substance (such as synthesis of organic substance, it is nitrogenous,
The rich nutritive material etc. of phosphorus) type and quantity be rapidly increasing, the pollution problem that water environment is faced is increasingly serious.Water resource
Pollution can not only restrict society sustainable development, seriously endanger the health and quality of life of people, more directly threat
The survival and development of the mankind, the improvement of water pollution be one of the matter of utmost importance that 21 century global environment resource faces.
In existing water treatment technology, absorption method due to easy to operate, material be easily obtained and application field it is wide and
It is widely applied.It is especially proposed in recent years using agricultural wastes such as stalk, coconut husk, corncobs as Material synthesis carbon
The method of matter adsorbent further reduces the production cost of adsorbent material.But traditional adsorbent material is merely by object
Pollutant in water has been transferred in adsorbent by the mode of reason absorption, does not realize the elimination of pollutant fundamentally, meanwhile,
Due to the difficulty of the pollutant subsequent processing in adsorbent, also results in adsorbent and be difficult to the shortcomings that reusing.On the other hand,
The photocatalytic degradation of based oxide semiconductor material photoelectric properties is also one received significant attention in current water treatment technology
Class method.Photocatalyst generated freely electricity under the excitation of the light of specific wavelength using oxide semiconductor material
The oxidation reaction of muonic catalysis organic matter makes organic pollutant be decomposed into the small molecules such as water, carbon dioxide, realizes to organic pollutant
Completely remove, meanwhile, the oxide semiconductor material as catalyst is also reusable.Further, since can use too
Sunlight can significantly reduce energy consumption in water treatment procedure, realize the target of energy-saving and emission-reduction as excitation light source, the technology.But
It is that the photocatalysis performance of oxide semiconductor material depends on its photoelectronic yield, the partial size for reducing material is to improve photoelectricity
One of the effective way of sub- yield, therefore, common photochemical catalyst is usually nano-powder.And the catalyst of powder morphology is in reality
There are the problems such as easy to reunite, recycling is difficult in the application of border, more there is the hidden danger for causing secondary pollution.To solve in existing water treatment technology
The problems of, traditional adsorbent material is combined with catalysis material, is made using the adsorbent material with high-specific surface area
For the carrier of nano-powder catalysis material, not only it is expected to improve the practical value of nano-photocatalyst material, is also expected to utilize light
Catalysis material realizes the reusable of adsorbent material to the degradation capability of organic matter.
Summary of the invention
The present invention proposes a kind of carbonization peanut shell load nano-titanium dioxide material and preparation method thereof, it is therefore intended that solves
In current water treatment technology, simple adsorbent material and the undesirable problem of simple catalysis material practical effect.Meanwhile this
The hydro-thermal reaction method of bio-fuel will be usually used in preparing in invention at present instead of commonly heating is split in current biomass carbonization
Solution is used for the carbonisation of peanut shell.Compared with heating cracking process, hydro-thermal reaction to the conservation rate of carbon in biomass compared with
Height also can preferably keep the original microstructure of biomass under the appropriate reaction conditions, so that being formed has higher ratio
The char-forming material of surface area；On the other hand, compared to the heating cracking reacted in the gas phase, hydrothermal carbonization is due in aqueous Jie
It is reacted in matter, acquired char-forming material surface is rich in hydroxyl, and carboxyl isoreactivity functional group can be as load other materials
The binding performance between institute support materials and char-forming material is improved in the site being surface modified.Therefore, heretofore described side
The carbonization peanut shell load nano-titanium dioxide material of method preparation is compared with existing carbon/oxide composite, in water
The degradation efficiency of organic dyestuff and the stability in reuse etc. have significant advantage.In addition, in the present invention
The preparation method of carbonization peanut shell load nano-titanium dioxide material, on the one hand using discarded peanut shell as raw material, source is wide
It is general to be easy to get, and can realize the environmental objective of the treatment of wastes with processes of wastes against one another, on the other hand by the carbonisation of biomass and oxide photocatalysis material
The synthesis process of material is combined into one, and preparation process is simple and easy.
The present invention adopts the following technical scheme:
A kind of preparation method for the peanut shell load nano-titanium dioxide material that is carbonized, comprising the following steps:
(1) peanut shell is milled and is cleaned with deionized water and impregnate certain time in the aqueous solution for be placed on titanium sulfate；
(2) in the mixed solution of the peanut shell and titanium sulfate, it is alkalinity that potassium hydroxide solution, which is added, and adjusts pH；
(3) peanut shell after the adjusting pH is transferred in hydrothermal reaction kettle with titanium sulfate mixed liquor, heat anti-
It answers, reaction solution is then obtained into solid by suction filtration, the solid is washed by washing, alcohol, then be dried to constant weight to obtain carbonization flower
Raw shell load nano-titanium dioxide material.
In above-mentioned technical proposal, in step (1), it is described mill after peanut shell partial size be 1~2mm.
In above-mentioned technical proposal, in step (1), dip time of the peanut shell in titanium sulfate aqueous solution be 30~
60min。
In above-mentioned technical proposal, in step (2), the concentration of the titanium sulfate solution is 0.03~0.04mol/L；The flower
It is 1: 1~5: 1 that the additional amount of raw shell, which is pressed with the mass ratio of titanium sulfate,.
In above-mentioned technical proposal, in step (2), the pH value of the mixed liquor after potassium hydroxide solution is adjusted is 8~10.
In above-mentioned technical proposal, in step (3), the temperature of the hydro-thermal reaction is 220~250 DEG C, the time is 12~
18h。
The carbonization peanut shell load of the preparation method preparation of present invention carbonization peanut shell load nano-titanium dioxide material is received
It is 20~40% that the nano-titanium dioxide partial size loaded in rice titanic oxide material, which is 10~50nm load capacity,.
Carbonization peanut shell load nano-titanium dioxide material in the present invention can be used for the organic dyestuff in water removal, tool
Body operating method is as follows:
A certain amount of carbonization peanut shell load nano-titanium dioxide material is taken, is added in the water containing organic dyestuff, by institute
It states mixed liquor and is placed under ultraviolet lighting and persistently stir.After a certain period of time, carbonization peanut shell is loaded by nanometer titanium dioxide by centrifugation
Titanium is separated from the water, and is measured using concentration of the ultraviolet spectrophotometry to Organic substance in water.Separating obtained carbonization peanut
Shell load nano-titanium dioxide material is reusable after distilled water cleaning and oven drying.
The beneficial effects of the present invention are:
After the present invention mixes peanut shell with the aqueous solution of titanium sulfate, the carbon of peanut shell is realized by one step of hydro-thermal reaction
Change and nano-titanium dioxide is in the load being carbonized in peanut shell, the carbonization peanut shell load nano-titanium dioxide material of preparation is simultaneously
Have the photocatalysis performance of the good characterization of adsorption of carbonization peanut shell and nano-titanium dioxide, thus overcomes general carbonaceous
Adsorbent material, which is difficult to reuse, is difficult to the shortcomings that recycling with nano-titanium dioxide powder, can effectively improve organic dirt in water
The removal efficiency of object is contaminated, processing cost is reduced.Meanwhile raw material used in the present invention is derived from discarded peanut shell, realizes pair
The resource utilization of agricultural wastes, carbon emission caused by reducing because of agricultural wastes embody the ring of " treatment of wastes with processes of wastes against one another "
Factoring is read.
Detailed description of the invention
Fig. 1 is (a) prepared by the present invention carbonization peanut shell load nano-titanium dioxide material and (b) carbonization peanut shell load
The scanning electron microscope (SEM) photograph of nanometer titanic oxide material part high magnification.
Fig. 2 is the X of (a) prepared by the present invention carbonization peanut shell load nano-titanium dioxide material and (b) carbonization peanut shell
X ray diffraction map.
Fig. 3 is the heat of (a) prepared by the present invention carbonization peanut shell load nano-titanium dioxide material and (b) carbonization peanut shell
Weight analysis map.
Fig. 4 is carbonization peanut shell load nano-titanium dioxide material, carbonization peanut shell and nano-silica prepared by the present invention
Change titanium powder to the degradation rate of water Methylene Blue.
Fig. 5 be carbonization peanut shell load nano-titanium dioxide material prepared by the present invention under the conditions of recycling in water
The degradation rate of methylene blue.
Specific embodiment
The present invention will be further described with specific embodiment with reference to the accompanying drawings of the specification.
Embodiment 1:
The preparation of carbonization metaplasia shell load nano-titanium dioxide material
It takes a certain amount of peanut shell to be milled and is crushed to 1~2mm, smashed peanut shell is stirred with deionized water by magnetic force
The mode mixed cleans 30min, the peanut shell after cleaning in an oven 60 DEG C of dryings to constant weight.
1g titanium sulfate is taken to be dissolved in 50mL deionized water, stirring to titanium sulfate is completely dissolved.Take 1g after being cleaned and dried
Peanut shell is added in titanium sulfate aqueous solution and persistently stirs 30min, takes saturation potassium hydroxide aqueous solution that titanium sulfate and flower is added dropwise
In the mixed solution of raw shell, pH value of solution is adjusted to 10.The mixed solution for regulating pH is transferred to the polytetrafluoro of hydrothermal reaction kettle
In ethylene liner, hydrothermal reaction kettle is screwed to fully sealed position.By hydrothermal reaction kettle as in baking oven, 250 DEG C of reaction 12h.
After reaction, by collected by suction solid product, respectively three times with deionized water and washes of absolute alcohol, then lead to
It crosses 60 DEG C of drying to constant weights of oven drying and obtains carbonization peanut shell load nano-titanium dioxide material.
Embodiment 2:
The preparation of carbonization peanut shell load nano-titanium dioxide material
It takes a certain amount of peanut shell to be milled and is crushed to 1~2mm, smashed peanut shell is stirred with deionized water by magnetic force
The mode mixed cleans 30min, the peanut shell after cleaning in an oven 60 DEG C of dryings to constant weight.
1g titanium sulfate is taken to be dissolved in 50mL deionized water, stirring to titanium sulfate is completely dissolved.Take 5g after being cleaned and dried
Peanut shell is added in titanium sulfate aqueous solution and persistently stirs 60min, takes saturation potassium hydroxide aqueous solution that titanium sulfate and flower is added dropwise
In the mixed solution of raw shell, pH value of solution is adjusted to 8.The mixed solution for regulating pH is transferred to the polytetrafluoroethyl-ne of hydrothermal reaction kettle
In alkene liner, hydrothermal reaction kettle is screwed to fully sealed position.By hydrothermal reaction kettle as in baking oven, 220 DEG C of reaction 18h.
After reaction, by collected by suction solid product, respectively three times with deionized water and washes of absolute alcohol, then lead to
It crosses 60 DEG C of drying to constant weights of oven drying and obtains carbonization peanut shell load nano-titanium dioxide material.
Embodiment 3:
Be carbonized degradation of the peanut shell load nano-titanium dioxide material to water Methylene Blue
It takes 0.02g methylene blue to be dissolved in deionized water, it is female to be transferred to the methylene blue that constant volume in 1L volumetric flask is 20mg/L
Liquid.Take 1,2,3,4,5mL methylene blue mother liquor respectively with pipette, as in 5 10mL volumetric flasks, with deionized water constant volume,
It is configured to the methylene blue standard solution that concentration is respectively 2,4,6,8,10mg/L.Using ultraviolet spectrophotometry in wavelength
The absorbance of methylene blue standard solution is measured at 664nm, and draws the standard curve of aqueous solution of methylene blue.
1g carbonization peanut shell load nano-titanium dioxide material is taken, is added in 300mL methylene blue mother liquor.Mixed solution is first
First as in camera bellows and magnetic agitation is kept, to be balanced absorption 1h.During being somebody's turn to do, every 15min takes out one from mixed liquor
Quantitative liquid, by the centrifuge separation carbonization peanut shell load nano-titanium dioxide material of 4000rpm revolving speed, centrifugation gained is clear
Liquid measures the absorbance at 664nm wavelength by ultraviolet specrophotometer, and passes through the standard curve meter of aqueous solution of methylene blue
Calculate the concentration of its Methylene Blue.After the completion of absorption, mixed solution is transferred under the ultraviolet lamp of 250W, continuing magnetic force stirring
2h, and a certain amount of liquid is taken out from mixed solution when 10,20,30,45,60,90,120min, pass through 4000rpm
The centrifuge separation carbonization peanut shell load nano-titanium dioxide material of revolving speed, centrifugation gained clear liquid pass through ultraviolet specrophotometer and survey
Determine the absorbance at 664nm wavelength, and calculates the concentration of its Methylene Blue by the standard curve of aqueous solution of methylene blue.Instead
Carbonization peanut shell load nano-titanium dioxide material is calculated after answering to the removal rate of Methylene Blue in Solution.
After reaction, carbonization peanut shell load nano-titanium dioxide material is separated by filtering, uses deionized water respectively
With washes of absolute alcohol three times after, cross 60 DEG C of dryings of oven drying to constant weight.Above-mentioned experimentation is pressed again, and 7 realities are repeated
It tests, removal rate of the carbonization peanut shell load nano-titanium dioxide material to Methylene Blue in Solution under the conditions of investigation is recycled.
Comparative example 1
The preparation of carbonization peanut shell
It takes a certain amount of peanut shell to be milled and is crushed to 1~2mm, smashed peanut shell is stirred with deionized water by magnetic force
The mode mixed cleans 30min, and the peanut shell after cleaning is added after filtering separation.In 50mL deionized water, saturation hydroxide is taken
Aqueous solutions of potassium is added dropwise in peanut shell and the mixed liquor of deionized water, adjusts pH value of solution to 10.The mixing for regulating pH is molten
Liquid is transferred in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, screws hydrothermal reaction kettle to fully sealed position.By hydro-thermal reaction
Kettle is as in baking oven, 250 DEG C of reaction 12h.
After reaction, by collected by suction solid product, respectively three times with deionized water and washes of absolute alcohol, then lead to
It crosses 60 DEG C of drying to constant weights of oven drying and obtains carbonization peanut shell.
Comparative example 2
Be carbonized removal of the peanut shell to water Methylene Blue
It takes 0.02g methylene blue to be dissolved in deionized water, it is female to be transferred to the methylene blue that constant volume in 1L volumetric flask is 20mg/L
Liquid.Take 1,2,3,4,5mL methylene blue mother liquor respectively with pipette, as in 5 10mL volumetric flasks, with deionized water constant volume,
It is configured to the methylene blue standard solution that concentration is respectively 2,4,6,8,10mg/L.Using ultraviolet spectrophotometry in wavelength
The absorbance of methylene blue standard solution is measured at 664nm, and draws the standard curve of aqueous solution of methylene blue.
1g carbonization peanut shell is taken, is added in 300mL methylene blue mother liquor.Mixed solution is first as in camera bellows and keeping magnetic
Power stirring, to be balanced absorption 1h, during being somebody's turn to do, every 15min takes out a certain amount of liquid from mixed liquor, passes through
The centrifuge separation carbonization peanut shell of 4000rpm revolving speed, centrifugation gained clear liquid are measured at 664nm wavelength by ultraviolet specrophotometer
Absorbance, and calculate by the standard curve of aqueous solution of methylene blue the concentration of its Methylene Blue.After the completion of absorption, it will mix
It closes solution to be transferred under the ultraviolet lamp of 250W, continuing magnetic force stirs 2h, and when 10,20,30,45,60,90,120min
A certain amount of liquid is taken out from mixed solution, passes through the centrifuge separation carbonization peanut shell of 4000rpm revolving speed, centrifugation gained clear liquid
The absorbance at 664nm wavelength is measured by ultraviolet specrophotometer, and is calculated by the standard curve of aqueous solution of methylene blue
The concentration of its Methylene Blue.Carbonization peanut shell is calculated after reaction to the removal rate of Methylene Blue in Solution.
Comparative example 3
Removal of the nano titanium dioxide powder to water Methylene Blue
It takes 0.02g methylene blue to be dissolved in deionized water, it is female to be transferred to the methylene blue that constant volume in 1L volumetric flask is 20mg/L
Liquid.Take 1,2,3,4,5mL methylene blue mother liquor respectively with pipette, as in 5 10mL volumetric flasks, with deionized water constant volume,
It is configured to the methylene blue standard solution that concentration is respectively 2,4,6,8,10mg/L.Using ultraviolet spectrophotometry in wavelength
The absorbance of methylene blue standard solution is measured at 664nm, and draws the standard curve of aqueous solution of methylene blue.
1g nano titanium dioxide powder is taken, is added in 300mL methylene blue mother liquor.Mixed solution first as in camera bellows simultaneously
Magnetic agitation is kept, to be balanced absorption 1h, during being somebody's turn to do, every 15min takes out a certain amount of liquid from mixed liquor, passes through
The centrifuge separation nano titanium dioxide powder of 4000rpm revolving speed, centrifugation gained clear liquid measure 664nm by ultraviolet specrophotometer
Absorbance at wavelength, and calculate by the standard curve of aqueous solution of methylene blue the concentration of its Methylene Blue.Absorption is completed
Afterwards, mixed solution being transferred under the ultraviolet lamp of 250W, continuing magnetic force stirs 2h, and respectively at 10,20,30,45,60,90,
A certain amount of liquid is taken out when 120min from mixed solution, passes through the centrifuge separation nanometer titanium dioxide titanium valve of 4000rpm revolving speed
End, centrifugation gained clear liquid measures the absorbance at 664nm wavelength by ultraviolet specrophotometer, and passes through aqueous solution of methylene blue
Standard curve calculate the concentration of its Methylene Blue.Nano titanium dioxide powder is calculated after reaction to solution methylene
Blue removal rate.
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbonization peanut shell load nano-titanium dioxide material of above-mentioned preparation, and a is carbonization peanut
Shell load nano-titanium dioxide material, b are the picture of carbonization peanut shell load nano-titanium dioxide material part high magnification.
Fig. 2 is the X ray diffracting spectrum of above-mentioned carbonization peanut shell load nano-titanium dioxide material.Fig. 3 is that above-mentioned carbonization peanut shell is negative
The thermogravimetric analysis map of nanometer titanic oxide material and the peanut shell that is carbonized is carried, a is carbonization peanut shell load nano-titanium dioxide material
Material, b are carbonization peanut shell.
It can be seen that carbonization peanut shell load nano-titanium dioxide material is in loose porous structure in Fig. 1 a, has and be used for
Adsorb the good capacity of the organic substance in water and the carrier as nano material；It can be seen that carbonization peanut shell load in Fig. 1 b
The loose and porous structure of nanometer titanic oxide material is made of many layer structures, this structure, which is conducive to improve it, compares table
There is a facilitation in face for its absorption and load capacity.
It can be seen that carbonization peanut shell load nano-titanium dioxide material is rendered as anatase in X-ray diffraction in Fig. 2 a
The typical map of type titanium dioxide, well-crystallized；It can be seen that carbonization peanut shell is not significant in X-ray diffraction in Fig. 2 b
Diffraction maximum, be showed only as the amorphous diffraction of carbon material, this result can also indirect proof nano-titanium dioxide loaded
In prepared carbonization peanut shell load nano-titanium dioxide material.
It can be seen that carbonization peanut shell load nano-titanium dioxide material is compared with the peanut shell that is carbonized in Fig. 3, nano-silica
The load capacity for changing titanium is 35%.
Fig. 4 is carbonization peanut shell load nano-titanium dioxide material, carbonization peanut shell and nano-silica prepared by the present invention
Change titanium powder to the degradation rate of water Methylene Blue.Fig. 5 is that carbonization peanut shell load nano-titanium dioxide material is being recycled
Under the conditions of to the degradation rate of aqueous solution Methylene Blue.
It can be seen that carbonization peanut shell load nano-titanium dioxide material can reach in 15min in dark situation in Fig. 4
Adsorption equilibrium, adsorption process is 30% to the removal rate of methylene blue, and under ultraviolet irradiation condition, carbonization peanut shell loads nanometer
Titanic oxide material significantly improves the removal rate of methylene blue, is to the removal rate of the methylene blue in water in 120min
91%.Peanut shell be carbonized in dark situation, is 15% to the removal rate of methylene blue in 60min, it is right under ultraviolet irradiation condition
The removal rate of methylene blue does not significantly improve, and final removal rate is 40%.Nano titanium dioxide powder in dark situation,
It is 20% to the removal rate of methylenum careuleum in 60min, under ultraviolet irradiation condition, nano titanium dioxide powder removes methylene blue
Except rate significantly improves, final removal rate is 85%.From the above it can be proved that carbonization peanut shell prepared by the present invention is negative
It carries nanometer titanic oxide material to be combined together absorption with photocatalysis, the removal ability of organic dyestuff in water is significantly better than
Only has the simple carbonization peanut shell of adsorption capacity, while also the nano titanium dioxide powder than only having photo-catalysis capability has
More preferably degradation speed.
It can be seen that carbonization peanut shell load nano-titanium dioxide material is being recycled in 7 times, to the Asia in water in Fig. 5
The removal rate of methyl blue is respectively as follows: 95%, 92%, 89%, 88%, 88%, 86%, 84%.
Claims (8)
1. a kind of preparation method for the peanut shell load nano-titanium dioxide material that is carbonized, comprising the following steps:
(1) peanut shell is milled and is cleaned with deionized water and impregnate certain time in the aqueous solution for be placed on titanium sulfate；
(2) in the mixed solution of the peanut shell and titanium sulfate, it is alkalinity that potassium hydroxide solution, which is added, and adjusts pH；
(3) peanut shell after the adjusting pH is transferred in hydrothermal reaction kettle with titanium sulfate mixed liquor, carries out heating reaction, so
Reaction solution is obtained into solid by suction filtration afterwards, the solid is washed by washing, alcohol, then be dried to constant weight to obtain carbonization peanut shell negative
Carry nanometer titanic oxide material.
2. the preparation method for the peanut shell load nano-titanium dioxide material that is carbonized according to claim 1, which is characterized in that step
Suddenly in (1), it is described mill after peanut shell partial size be 1~2mm.
3. the preparation method for the peanut shell load nano-titanium dioxide material that is carbonized according to claim 1, which is characterized in that step
Suddenly in (1), dip time of the peanut shell in titanium sulfate aqueous solution is 30~60min.
4. the preparation method for the peanut shell load nano-titanium dioxide material that is carbonized according to claim 1, which is characterized in that step
Suddenly in (2), the concentration of the titanium sulfate solution is 0.03~0.04mol/L；The additional amount of the peanut shell is pressed and titanium sulfate
Mass ratio is 1: 1~5: 1.
5. the preparation method for the peanut shell load nano-titanium dioxide material that is carbonized according to claim 1, which is characterized in that step
Suddenly in (2), the pH value of the mixed liquor after potassium hydroxide solution is adjusted is 8~10.
6. the preparation method for the peanut shell load nano-titanium dioxide material that is carbonized according to claim 1, which is characterized in that step
Suddenly in (3), the temperature of the hydro-thermal reaction is 220~250 DEG C, and the time is 12~18h.
7. the carbonization peanut of the preparation method preparation for the peanut shell load nano-titanium dioxide material that is carbonized according to claim 1
Shell load nano-titanium dioxide material.
8. be carbonized peanut shell load nano-titanium dioxide material according to claim 7, which is characterized in that the nano-silica
Change titanium partial size is 10~50nm；The load capacity of the nano-titanium dioxide is 20~40%.
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