CN110237812A - A kind of biomass carbon modification selenizing molybdenum nano material, preparation method and its application - Google Patents
A kind of biomass carbon modification selenizing molybdenum nano material, preparation method and its application Download PDFInfo
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Abstract
The present invention relates to a kind of biomass carbon modification selenizing molybdenum nano material, preparation method and its applications, the nano material includes the selenizing molybdenum nano material of 2 mass %-10 mass % unformed biomass carbon particle and surplus, and unformed biomass carbon particle is grown in selenizing molybdenum nanometer sheet surface.Preparation method is: biomass waste material is obtained biomass carbon particle by zinc acetate solution infiltration, drying and calcination；Resulting biomass carbon particle is distributed in water, soluble molybdenum salt, selenium powder, reducing agent and surfactant is added, after sealing hydro-thermal reaction, obtains the modified selenizing molybdenum nanocomposite of biomass carbon.The present invention modifies the absorption property and power of regeneration of selenizing molybdenum raising active carbon by introducing biomass carbon, and can apply to the adsorption treatment of industrial wastewater.
Description
Technical field
The present invention relates to nano material and environment-friendly materials fields, specifically a kind of biomass carbon modifies selenizing molybdenum nanometer
The modification of material, preparation method and the renewable active carbon applied to formaldehyde adsorption.
Background technique
All the time, physisorphtion is considered as a wide range of solution air pollution and Non-aqueous processing most efficient method.
It has been obtained widely using active carbon as the conventional adsorbent of representative because of the advantage of its good physics, chemical property and low cost
Using, however its separation property difference and regenerative adsorption performance lower limit in water its further apply, therefore find novel
Nanoscale adsorbent material and modified traditional adsorbent are the research and development hot spots in current environment field.
Two-dimensional material headed by graphene, because its unique structure and due to excellent performance energy and environment field by
Extensive concern and application are arrived.Recent study report also demonstrates that the transition metal sulfoselenide of class graphene-structured is latent
Adsorbent material, the layer structure of S-M-S helps to promote its absorption property, has wide application in water treatment field
Prospect.In addition, application No. is CN 109569512 A, CN 109499532 A, CN 109364922 A Chinese patent application
File discloses the method for various modified commodity grade active carbons, to obtain more preferably absorption property and reproducible adsorbent.So
And the report that the modified selenizing molybdenum of biomass carbon is applied to sewage treatment is less.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of biomass carbons to modify selenizing molybdenum nanometer
Material modifies the absorption property and power of regeneration of selenizing molybdenum raising active carbon by introducing biomass carbon, and can apply to industry
The adsorption treatment of waste water.
It is another object of the present invention to provide a kind of preparation method of biomass carbon modification selenizing molybdenum nano material, works
Skill is simple, and yield is high.
It is yet a further object of the present invention to provide a kind of biomass carbon modification selenizing molybdenum Application of micron in absorption first
The modification of the renewable active carbon of aldehyde.
Foregoing invention purpose is achieved by the following technical solution:
Biomass carbon modifies selenizing molybdenum adsorbent material, including biomass carbon particle and selenizing molybdenum nano material, wherein biology
The content of matter charcoal be 2%-10%, surplus be selenizing molybdenum wherein.Moreover, unformed biomass carbon particle is grown in MoSe2It receives
Rice piece surface, unformed C particle mean size are 200nm.
The preparation method of biomass carbon modification selenizing molybdenum adsorbent material, comprising the following steps:
(1) it the preparation of biomass carbon: after biomass waste material is crushed, is cleaned, is dry, is soaked repeatedly by zinc acetate solution
Profit, drying and calcination obtain the product of black；Dilute hydrochloric acid solution is added in above-mentioned product and removes the oxidation generated in carburizing reagent
Zinc, then through repeatedly washing and being dried to obtain biomass carbon particle.The particle size of smashed biomass carbon is 200nm；
Carburizing temperature is 550-750 DEG C, soaking time 1-3h.
Biomass carbon raw material used is reproducible waste materials containing carbon, such as the waste of the fallen leaves of plant, deadwood and fruit, grass
The stalk of this plant.
Impregnation ratio is: biomass waste material dosage 20-50g, and the concentration of zinc acetate solution is 0.5-1mol/L.
The dilute hydrochloric acid solution concentration is 0.5mol/L.
(2) synthesis of the modified selenizing molybdenum of biomass carbon: by biomass carbon particle obtained in step (1) be distributed to from
In sub- water, it is then respectively adding soluble molybdenum salt, selenium powder, reducing agent and surfactant, after continuing stirring, it is anti-to move into stainless steel
Kettle is answered, is sealed, after incubation water heating reaction, is cooled to room temperature, by the multiple washing and drying of heat alkali liquid, ionized water and ethyl alcohol
Afterwards, the modified selenizing molybdenum nanocomposite of biomass carbon is obtained.
Soluble molybdenum salt used is ammonium molybdate, sodium molybdate, molybdenum pentachloride；
Reducing agent is hydroxylamine hydrochloride, sodium borohydride；
Heat alkali liquid is sodium hydroxide or potassium hydroxide solution, and concentration 1-3mol/L, the preferably NaOH of 0.2mol/L are molten
Liquid；Hydrothermal synthesis temperature is 180-240 DEG C.
Soluble molybdenum salt and selenium powder relationship: Mo:Se molar ratio is 1:2.1-2.4.
The relationship of soluble molybdenum salt and reducing agent: Mo6+:NaBH4Molar ratio is 1:0.5-0.4；Mo6+:NH2OHHCl rubs
You are than being 1:2-2.5.
The additive amount of surfactant in the solution is 0.04-0.12g/L.
Biomass carbon modifies selenizing molybdenum Application of micron in the modification of renewable active carbon, and steps are as follows:
(1) component of adsorbent material is as follows: the modified selenizing molybdenum nanocomposite 5-10% of biomass carbon, magnetic Nano
Grain 2-6%, diatom ooze 8-20%, surplus is active carbon；
The magnetic nanoparticle is iron-based oxide, such as Fe2O3、Fe3O4, crystal particle scale 50-300nm；
Active carbon is commerical grade, such as absorbent charcoal material is prepared in coconut husk, timber and coal carbon source.
(2) above-mentioned material is uniformly mixed, ethanol solution is auxiliary agent, and the slurry of 100-200 mesh is obtained after ball milling 4-8h, is washed
It washs after drying again through low temperature calcination 1-2h under 200-300 DEG C of isolation air conditions, renewable modified activated carbon adsorbent material is made.
The recycling of above-mentioned adsorbent material can fast implement the separation of adsorbent material and solution under the action of externally-applied magnetic field, return
Yield reaches 90-95%.
The regeneration method of above-mentioned renewable modified activated carbon adsorbent material is the modified activated carbon suction for being up to adsorption equilibrium
Enclosure material keeps constant temperature 1-2h under the conditions of 80-100 DEG C, and then under the conditions of nitrogen protection, temperature keeps 400-600 DEG C of desorption 1-
2h。
The renewable composite reactive carbon adsorbent is renewable twice using the regeneration method, the modified work after secondary recycling
Property charcoal adsorbent material adsorbance can reach the 70%~85% of former adsorbance.
The cost of the method for the present invention is inexpensive, and simple production process is easily-controllable, and product rate is high, is suitble to large-scale industry raw
It produces.
Detailed description of the invention
Fig. 1 is the obtained C@MoSe of the present invention2The EDS spectrogram of composite nano materials.Show product C@MoSe2By Mo, Se, C member
The element composition of synthetic product, without other impurity, Mo:Se 1:1.98 is consistent with chemical formula.
Fig. 2 is the obtained C@MoSe of the present invention2The scanning electron microscope (SEM) photograph (SEM) and transmission electron microscope picture (TEM) of composite nano materials.
Fig. 2 a is synthetic product C@MoSe2SEM figure, unformed C particle is grown in MoSe as seen from the figure2Nanometer sheet surface, TEM figure
(Fig. 2 b) further demonstrates that unformed C particle mean size is 200nm.
Specific embodiment
The present invention is further described below by way of specific embodiment, as known by the technical knowledge, the present invention can also pass through it
Its scheme for not departing from the technology of the present invention feature describes, therefore all within the scope of the present invention or in the equivalent scope of the invention
Change be included in the invention.
All reagents according to the present invention are commercial product.
Embodiment 1:
The synthesis of biomass carbon modification selenizing molybdenum nano material
(1) preparation of biomass carbon:
The dead leaf of 20g is crushed to the particle that diameter is 5mm, then washs drying through deionized water, dehydrated alcohol；
Above-mentioned particle is added to the ZnAC of 0.5mol/L2Solution infiltrates 3 times repeatedly, then in an oven after 80 DEG C of dry 10h,
It is transferred in tube furnace in 550 DEG C of heat preservation 2h, completely cuts off under air conditions and be carbonized, after being cooled to room temperature；
It is washed 3 times after reaction product is successively washed with the HCl solution of 0.5mol/L, deionization hydration dehydrated alcohol, it is dry
Biomass carbon is obtained afterwards.
(2) the biomass carbon 0.026g synthesized in (1) is distributed in the deionized water of 50mL, then by 1.21g
Na2MoO4·2H2O, 0.869g Se powder, 0.19g NaBH4It is added in above-mentioned suspension, is transferred to after magnetic agitation 30min
In 100mL stainless steel cauldron, it is placed in vacuum oven and is cooled to room temperature after keeping the temperature 6h at 200 DEG C.
The black product of preparation is transferred to the NaOH solution of 50mL 0.2mol/L, is transferred to baking oven after magnetic agitation 10min
In 80 DEG C of heat preservation 2h to remove extra Se, then after cooled to room temperature, be filtered, washed and dried drying, obtain biomass carbon
Modify selenizing molybdenum nano material.
The preparation of renewable modified activated carbon absorbent
By weight percentage, the modified selenizing molybdenum nanocomposite 5% of biomass carbon, Fe2O3Nano particle 2%, diatom
Above-mentioned magnetic agitation 2h is uniformly mixed it by mud 8%, active carbon 85%, and ethyl alcohol is auxiliary agent, and quality is added material
Renewable modified active is made again through low temperature calcination 1h under 200 DEG C of isolation air conditions in washed drying again after 5%, ball milling 4h
Charcoal adsorbent material, the content of biomass carbon are 2%, and the content of selenizing molybdenum is 98%.
Embodiment 2:
The synthesis of biomass carbon modification selenizing molybdenum nano material
(1) preparation of biomass carbon: by the rice straw of 30g be crushed to diameter be 8mm particle, then through deionized water,
After dehydrated alcohol washing is dry, above-mentioned particle is added to the ZnAC of 1mol/L2Solution infiltrates 3 times repeatedly, then 80 DEG C in an oven
It after dry 10h, is transferred in tube furnace in 750 DEG C of heat preservation 1h, completely cuts off under air conditions and be carbonized, after being cooled to room temperature, reaction is produced
Object washs 3 times after successively being washed with the HCl solution of 0.5mol/L, deionization hydration dehydrated alcohol, obtains biomass carbon after dry.
(2) the biomass carbon 0.065g synthesized in (1) is distributed in the deionized water of 50mL, then by 1.21g
Na2MoO4·2H2O, 0.948g Se powder, 0.35g hydroxylamine hydrochloride are added in above-mentioned suspension, are transferred to after magnetic agitation 60min
In 100mL stainless steel cauldron, it is placed in vacuum oven and is cooled to room temperature after keeping the temperature 12h at 220 DEG C.The black of preparation is produced
Object is transferred to the NaOH solution of 50mL 0.2mol/L, and it is extra to remove that 80 DEG C of heat preservation 2h in baking oven are transferred to after magnetic agitation 10min
Se, then after cooled to room temperature, be filtered, washed and dried drying, obtain biomass carbon modification selenizing molybdenum nano material.
The preparation of renewable modified activated carbon absorbent:
By weight percentage, the modified selenizing molybdenum nanocomposite 10% of biomass carbon, magnetic nanoparticle 6%, silicon
Above-mentioned magnetic agitation 2h is uniformly mixed it by algal gel 20%, active carbon 64%, and ethyl alcohol is auxiliary agent, and quality is added material
8%, washed drying is made renewable modified living again through low temperature calcination 1h under 300 DEG C of isolation air conditions again after ball milling 8h
Property charcoal adsorbent material, the content of biomass carbon is 5%, and the content of selenizing molybdenum is 95%.
Embodiment 3:
The synthesis of biomass carbon modification selenizing molybdenum nano material
(1) preparation of biomass carbon: the bamboo of 50g is crushed to the particle that diameter is 6mm, then through deionized water, anhydrous
After ethanol washing is dry, above-mentioned particle is added to the ZnAC of 0.5mol/L2Solution infiltrates 3 times repeatedly, then in an oven 80 DEG C it is dry
After dry 10h, it is transferred in tube furnace in 650 DEG C of heat preservation 3h, completely cuts off under air conditions and be carbonized, after being cooled to room temperature, by reaction product
It is washed 3 times after successively being washed with the HCl solution of 0.5mol/L, deionization hydration dehydrated alcohol, obtains biomass carbon after dry.
(2) the biomass carbon 0.13g synthesized in (1) is distributed in the deionized water of 50mL, then by 1.365g MoCl5、
0.869g Se powder, 0.19g NaBH4It is added in above-mentioned suspension, 100mL stainless steel reaction is transferred to after magnetic agitation 30min
In kettle, it is placed in vacuum oven and is cooled to room temperature after keeping the temperature 6h at 200 DEG C.
The black product of preparation is transferred to the NaOH solution of 50mL 0.2mol/L, is transferred to baking oven after magnetic agitation 10min
In 80 DEG C of heat preservation 2h to remove extra Se, then after cooled to room temperature, be filtered, washed and dried drying, obtain biomass carbon
Selenizing molybdenum nano material is modified, the content of biomass carbon is 10%, and the content of selenizing molybdenum is 90%.
The preparation of renewable modified activated carbon absorbent
By weight percentage, the modified selenizing molybdenum nanocomposite 8% of biomass carbon, magnetic nanoparticle 4%, diatom
Above-mentioned magnetic agitation 2h is uniformly mixed it by mud 15%, active carbon 73%, and ethyl alcohol is auxiliary agent, and quality is added material
Renewable modified active is made again through low temperature calcination 1h under 250 DEG C of isolation air conditions in washed drying again after 5%, ball milling 6h
Charcoal adsorbent material.
Embodiment 4: test experiments
Using the organic dye content in Shimadzu UV-vis spectroscopy degree photometer (UV2550) measurement waste liquid, Shimadzu is former
Heavy metal ion content in sub- absorption spectrophotometer (AA-7000) measurement waste liquid.
Specifically, configuration organic dye solution, is then added acticarbon and city made from inventive embodiments 1-3
Sell active carbon, pH value 7, magnetic agitation rotating speed 200r/min, being tested using UV-vis spectroscopy degree photometer different is had
The amount of engine dyeing material after balance to be adsorbed, records adsorption saturation time, measures and calculate the maximal absorptive capacity of organic dyestuff.It is identical
, using the adsorption saturation time and maximal absorptive capacity of atomic absorption spectrophotometer measurement heavy metal ion.Specific data are shown in
Table 1:
The different embodiments of table 1 adsorb the index of different pollutions
As shown in Table 1, all embodiments are superior to the adsorption rate of organic dyestuff and heavy metal ion with adsorbance
Commercially available active carbon, therefore, the present invention are beneficial to improve the absorption property of active carbon, have beneficial effect.
Claims (8)
1. a kind of biomass carbon modifies selenizing molybdenum adsorbent material, which is characterized in that including unformed biomass carbon particle and selenium
Change molybdenum nano material, the content of unformed biomass carbon particle is 2 mass %-10 mass %, surplus be selenizing molybdenum wherein；Wherein
Unformed biomass carbon particle is grown in selenizing molybdenum nanometer sheet surface, and the average-size of unformed biomass carbon particle is
200nm。
2. the preparation method of biomass carbon as described in claim 1 modification selenizing molybdenum adsorbent material, which is characterized in that including with
Lower step:
(1) it the preparation of biomass carbon: after biomass waste material is crushed, is cleaned, is dry, is infiltrated repeatedly by zinc acetate solution, is dry
Dry and calcining obtains the product of black；Dilute hydrochloric acid solution is added in above-mentioned product and removes the zinc oxide generated in carburizing reagent, then
Repeatedly washed and be dried to obtain biomass carbon particle；
(2) biomass carbon particle obtained in step (1) synthesis of the modified selenizing molybdenum of biomass carbon: is distributed to deionized water
In, it is then respectively adding soluble molybdenum salt, selenium powder, reducing agent and surfactant, after continuing stirring, moves into stainless steel reaction
Kettle, sealing are cooled to room temperature after incubation water heating reaction, after the multiple washing and drying of heat alkali liquid, ionized water and ethyl alcohol,
Obtain the modified selenizing molybdenum nanocomposite of biomass carbon.
3. the preparation method of biomass carbon modification selenizing molybdenum adsorbent material as claimed in claim 2, which is characterized in that step
(1) in, impregnation ratio is: biomass waste material dosage 20-50g, and the concentration of zinc acetate solution is 0.5-1mol/L；
Carburizing temperature is 550-750 DEG C, soaking time 1-3h；Biomass carbon raw material used is reproducible waste materials containing carbon.
4. the preparation method of biomass carbon modification selenizing molybdenum adsorbent material as claimed in claim 2, which is characterized in that step
(2) in, soluble molybdenum salt used is ammonium molybdate, sodium molybdate or molybdenum pentachloride；Reducing agent is hydroxylamine hydrochloride, sodium borohydride；Heat
Lye is sodium hydroxide or potassium hydroxide solution, and concentration 1-3mol/L, hydrothermal synthesis temperature is 180-240 DEG C.
5. the preparation method of biomass carbon modification selenizing molybdenum adsorbent material as claimed in claim 4, which is characterized in that soluble
Molybdenum salt and selenium powder relationship: Mo:Se 1:2.1-2.4；The relationship of soluble molybdenum salt and reducing agent: Mo6+:NaBH4Molar ratio is 1:
0.5-0.4；Mo6+:NH2OHHCl molar ratio is 1:2-2.5；The additive amount of surfactant in the solution is 0.04-0.12g/
L。
6. biomass carbon modification selenizing molybdenum adsorbent material is used to prepare renewable modified activated carbon adsorbent material.
7. biomass carbon modification selenizing molybdenum adsorbent material as claimed in claim 6 is used to prepare renewable modified activated carbon absorption
Material, which is characterized in that steps are as follows:
(1), it is mixed according to following mass percent: the modified selenizing molybdenum nanocomposite 5-10% of biomass carbon, magnetic Nano
Particle 2-6%, diatom ooze 8-20%, surplus are active carbon；
(2), using ethanol solution as auxiliary agent, the slurry of 100-200 mesh is obtained after ball milling, after washing is dry again through 200-300 DEG C every
Low temperature calcination 1-2h under exhausted air conditions, is made renewable modified activated carbon adsorbent material.
8. biomass carbon modification selenizing molybdenum adsorbent material as claimed in claim 6 is used to prepare renewable modified activated carbon absorption
Material, which is characterized in that the magnetic nanoparticle is Fe2O3Or Fe3O4, crystal particle scale 50-300nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111097381A (en) * | 2019-12-02 | 2020-05-05 | 镇江市高等专科学校 | Renewable modified activated carbon adsorbent and preparation method and application thereof |
| CN111420684A (en) * | 2020-03-26 | 2020-07-17 | 内蒙古大学 | Catalyst for directly preparing ethanol from synthesis gas and application thereof |
| CN111777056A (en) * | 2020-07-13 | 2020-10-16 | 南昌航空大学 | Hydrated carbon/amorphous molybdenum selenide composite material and preparation method and application thereof |
| CN114920212A (en) * | 2022-06-14 | 2022-08-19 | 蚌埠学院 | Preparation method and application of molybdenum selenide nano material |
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| CN116870866A (en) * | 2023-08-07 | 2023-10-13 | 昆明理工大学 | Preparation method and application of coffee grounds biomass composite material |
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