CN110052242A - A kind of load carbon quantum dot/W18O49The preparation method of the renewable porous carbon adsorbent of photocatalysis - Google Patents
A kind of load carbon quantum dot/W18O49The preparation method of the renewable porous carbon adsorbent of photocatalysis Download PDFInfo
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- CN110052242A CN110052242A CN201910342029.0A CN201910342029A CN110052242A CN 110052242 A CN110052242 A CN 110052242A CN 201910342029 A CN201910342029 A CN 201910342029A CN 110052242 A CN110052242 A CN 110052242A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3441—Regeneration or reactivation by electric current, ultrasound or irradiation, e.g. electromagnetic radiation such as X-rays, UV, light, microwaves
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
The invention discloses a kind of load carbon quantum dot/W18O49The preparation method of the renewable porous carbon adsorbent of photocatalysis, is related to technical field of material, this method comprises: (1) furfural waste-water carries out hydro-thermal reaction, resulting precursor carbon material KOH aqueous solution soaking, calcining obtains porous carbon adsorbent；(2) citric acid mixes hydro-thermal reaction with urea, dialyses, is lyophilized after filtering, obtains carbon quantum dot, carbon quantum dot ethanol solution is made；(3) by WCl6It is dissolved in dehydrated alcohol into mixture and polyethylene glycol, carbon quantum dot ethanol solution and porous carbon adsorbent is added, hydro-thermal reaction, isolated load carbon quantum dot/W18O49The renewable porous carbon adsorbent of photocatalysis.The present invention realized using the above method recycling of furfural waste-water, wastewater containing phenol be effectively treated and the Photocatalytic Regeneration of porous carbon materials recycles, have good production application value.
Description
Technical field
The present invention relates to technical field of material, and in particular to a kind of furfural wastewater with high concentration prepares porous as carbon source
Carbon loads carbon quantum dot/W18O49The method of photochemical catalyst preparation regenerable sorbent.
Background technique
With the rapid development of the national economy, the phenol as important industrial chemicals is widely used in oil refining, coal conversion, stone
The industries such as oiling work, medicine, pesticide, due to phenol have carcinogenicity, teratogenesis and difficult for biological degradation, wastewater containing phenol without
Processing, which is discharged into environment, seriously threatens human health.Currently, wastewater containing phenol is treated as the hot issue of sewage treatment field,
Porous carbon materials absorption because its have the advantages that it is efficient, easy to operate and recyclable due to receive significant attention, but porous carbon
Material is conducive to the absorption to organic pollutant because of its large aperture and high-specific surface area, and problem regenerates difficulty after being adsorption saturation
Can not secondary use, the solid waste of generation is directly discharged to will cause serious secondary pollution in environment, and it is high to be not suitable for processing
The phenolic waste water of concentration；And porous carbon materials mostly use greatly coal, petroleum, biomass etc. to be prepared, preparation process energy consumption height is simultaneously
And release pernicious gas, it is unfavorable for environmental protection and energy saving.
Material with near-infrared (NIR) shielding character, especially transition metal oxide nano structure gradually cause to learn
The concern of person.W18O49Photochemical catalyst has very strong, tunable local within the scope of the near-infrared wavelength of 780-2526nm
Plasma resonance effect, therefore there are good absorbing properties, still, pure W for the near infrared region of sunlight18O49
Electron hole is easily compound in fault location in photochemical catalyst use, greatly reduces photocatalytic activity.
Summary of the invention
To solve the above problems, the present invention provides a kind of load carbon quantum dot/W18O49The renewable porous carbon of photocatalysis is inhaled
Attached dose of preparation method, comprising the following steps:
(1) preparation of porous carbon materials: furfural wastewater with high concentration carries out hydro-thermal reaction, filters to take solid, obtains precursor carbon
Material is dried with KOH aqueous solution soaking, and calcining obtains the porous carbon adsorbent using furfural wastewater with high concentration as carbon source；
(2) preparation of carbon quantum dot: citric acid mixes hydro-thermal reaction with urea, after being cooled to room temperature, uses needle type filtration
Device filtering, filtered filtrate dialysis, acquired solution freeze-drying obtain carbon quantum dot；Gained carbon quantum dot is dissolved in dehydrated alcohol,
Carbon containing quantum dot 0.05g, obtains carbon quantum dot ethanol solution in 10mL solution；
(3) carbon quantum dot/W is loaded18O49The preparation of the renewable porous carbon adsorbent of photocatalysis: by WCl6It is dissolved in anhydrous second
(by WCl in alcohol6It is added to absolute ethanol to be placed on magnetic stirring apparatus and be vigorously stirred, until WCl6It is dissolved completely in dehydrated alcohol
In), the porous carbon of polyethylene glycol, the carbon quantum dot ethanol solution of step (2) preparation and step (1) preparation is added into mixture
Adsorbent is added in pyroreaction kettle, hydro-thermal reaction after mixing, and gained mixture separation after reaction obtains load carbon amounts
Sub- point/W18O49The renewable porous carbon adsorbent of photocatalysis.
Step (1) described furfural wastewater with high concentration, for the furfural under the primary distillation tower for the furfural for being 15% containing volume fraction
Waste water.
Step (1) described hydro-thermal reaction, reaction temperature are 200 DEG C, reaction time 8h.
The concentration of step (1) the KOH aqueous solution is 1.12g/mL；Soaking time is 10-18h.
Step (1) described calcining, carries out under nitrogen protection, and heating rate is 3 DEG C/min, and calcination temperature is 800 DEG C,
The calcining at constant temperature time is 1h at 800 DEG C.
The mass ratio of step (2) citric acid and urea is 1:4.
Step (2) described hydro-thermal reaction, reaction temperature are 160 DEG C, reaction time 6h.Reaction vessels are polytetrafluoroethylene (PTFE)
Reaction kettle.
Step (2) the syringe filter filter sizes are 0.22 μm.
Step (2) described dialysis, is dialysed using bag filter, through molecular weight 500-100Da.
Step (3) described WCl6Concentration in dehydrated alcohol is 0.005g/mL, the WCl6Quality and polyethylene glycol
The ratio between volume be 1:100g/mL, the volume ratio of polyethylene glycol and carbon quantum dot ethanol solution is 2:1, porous carbon adsorbent
The ratio between quality and the volume of carbon quantum dot ethanol solution 1:10g/mL；
It is PPL (polyparaphenylene phenol) liner pyroreaction kettle in step (3) described pyroreaction kettle.
Step (3) described hydro-thermal reaction, reaction temperature are 240 DEG C, reaction time 20h.
Step (3) described separation, specifically: the centrifugation of gained mixture, after taking precipitating, precipitating to rinse resuspension with dehydrated alcohol
Centrifuging and taking precipitates and repeats this operation twice, and gained is dried in vacuo under the conditions of precipitating 70 DEG C.
Beneficial effect
Firstly, the present invention prepares porous carbon adsorbent using furfural wastewater with high concentration as carbon source, high concentration chaff is realized
The recycling of aldehyde waste water has reached recycling, handling high concentration phenol waste water, protection environment and control pollution for adsorbent
Purpose.
Second, the present invention utilizes W18O49After photochemical catalyst and carbon quantum dot are compound, the charge migration of carbon quantum dot is improved
Rate, allow the light induced electron in carbon quantum dot more quickly and effectively be transferred to W18O49Photocatalyst surface, to improve
Its separation of charge rate, further improves catalytic activity.By carbon quantum dot/W18O49Photocatalyst material, which is supported on, have been prepared
Out on porous carbon adsorbent, load carbon quantum dot/W has been prepared18O49The renewable porous carbon adsorbent of photocatalysis has good
Stability and Photocatalytic Regeneration ability, Pyrogentisinic Acid's waste water have good adsorption effect.
For synthesis, the present invention prepares porous carbon materials using furfural wastewater with high concentration and loads carbon quantum dot/W18O49Light
Catalyst material preparation has load carbon quantum dot/W of renewable performance18O49The renewable porous carbon adsorbent of photocatalysis solves
Existing pure W18O49Photochemical catalyst does not have the absorption and photocatalytic degradation capability of stronger Pyrogentisinic Acid under near infrared light, passes
Unite absorbent charcoal material Pyrogentisinic Acid adsorption effect it is poor, without regenerability, can be recycled problem.The present invention realizes
The recycling of furfural wastewater with high concentration, wastewater containing phenol be effectively treated and the Photocatalytic Regeneration of porous carbon materials circulation benefit
With with good production application value.Utilize carbon quantum dot/W18O49Photocatalyst material is carried on porous carbon materials, is risen
It is regenerated to using porous carbon materials of the photocatalysis to adsorption saturation, the adsorbent of realization recycles.Carbon quantum
The addition of point improves the separative efficiency of light induced electron, promotes electron hole separation, to make W18O49Photochemical catalyst has more preferable
Photocatalysis performance, and W can be made18O49Crystal preferably crystallizes in porous carbon materials surface and aperture, improves compound effect
Rate.Absorption result compares it is found that three-phase composite sample loads carbon quantum dot/W18O49The renewable porous carbon adsorbent of photocatalysis with
Pure W18O49Photochemical catalyst, carbon quantum dot/W18O49Three kinds of photocatalyst material, porous carbon adsorbent samples are compared, and absorption property has
It is certain to be promoted, to the removal efficiency of 500mg/L phenol up to 80% or more after 180min.And absorption power is carried out to sample
Learn the research with adsorption isotherm, samples met puppet secondary absorption dynamics and langmuir's adsorption isotherm.Prepared
Adsorbent has preferable treatment effect for high concentration phenol waste water, and can be regenerated by light-catalysed mode.
It is preferable to illustrate that sample has no more than 6% for the difference that the regeneration test that five circulations are carried out to it can be seen that its absorption property
Regenerability.
Detailed description of the invention
The absorption property of tetra- kinds of material Pyrogentisinic Acids of Fig. 1 compares figure；
Phenol concentration change curve of the tetra- kinds of materials of Fig. 2 in 5 circulating repetition experimentations；
Fig. 3 loads carbon quantum dot/W18O49The renewable porous carbon adsorbent Sample Scan electron microscope of photocatalysis；Figure a is low power
Figure, figure b are high power figure；
Fig. 4 loads carbon quantum dot/W18O49The transmission electron microscope picture of the renewable porous carbon adsorbent of photocatalysis；Figure a is low power figure
And partial enlarged view, figure b are high power figure.
Specific embodiment
Embodiment 1 loads carbon quantum dot/W18O49The preparation of the renewable porous carbon adsorbent of photocatalysis:
(1) preparation of porous carbon materials: furfural wastewater with high concentration prepares precursor carbon material as utilization of carbon source hydro-thermal method, high
Concentration furfural waste-water hydro-thermal reaction 8h under the conditions of 200 DEG C of temperature, and the precursor carbon material prepared progress KOH activation is made
Carbon material has bigger specific surface area and adsorption capacity, by the precursor carbon material after impregnating KOH and drying in N2Under protection
800 DEG C of calcining, heating rate are 3 DEG C/min, and calcining at constant temperature 1h obtains the suction of the porous carbon using furfural wastewater with high concentration as carbon source
Attached dose；
The furfural wastewater with high concentration, for the furfural waste-water under the primary distillation tower for the furfural for being 15% containing volume fraction；
The concentration of the KOH aqueous solution is 1.12g/mL；Soaking time is 10h.
(2) in the ptfe autoclave of 50mL, 1g citric acid, 4g urea the preparation of carbon quantum dot: is added.In temperature
Under the conditions of degree is 160 DEG C, hydro-thermal reaction 6h.After being cooled to room temperature, supernatant is absorbed and filter using pin hole filter, using 0.22
μm filter sizes, after filtering using bag filter dialysis (molecular weight: 500-100Da) obtain carbon quantum dot (CD), by carbon quantum
Point is dissolved in dehydrated alcohol, and carbon containing quantum dot 0.05g in every 10mL solution obtains carbon quantum dot ethanol solution.
(3) carbon quantum dot/W is loaded18O49The preparation of the renewable porous carbon adsorbent of photocatalysis: by the WCl of 0.2g6It is dissolved in
It is placed on magnetic stirring apparatus and is vigorously stirred in 40mL dehydrated alcohol, WCl6After being dissolved completely in dehydrated alcohol, into mixture
The carbon quantum dot ethanol solution of 20mL polyethylene glycol (PEG) and 10mL step (2) preparation are imported, then is put into 1.0g step (1)
Prepared porous carbon adsorbent continues to stir, and PPL (polyparaphenylene phenol) the liner high temperature for being packed into 100mL after mixing is anti-
It answers in kettle, hydro-thermal process 20h under conditions of temperature is 240 DEG C.Mixture in reaction kettle is centrifuged after reaction, after retaining centrifugation
Blue solid, and with dehydrated alcohol repeated flushing be centrifuged 3 times, remove product in organic impurities.Finally gained is consolidated
Body is dried in vacuo under the conditions of 70 DEG C obtains load carbon quantum dot/W18O49Photocatalysis renewable porous carbon adsorbent (abbreviation carbon
Quantum dot/W18O49/ carbon).
Comparative example
(3) pure W18O49Photochemical catalyst and carbon quantum dot/W18O49The preparation of photocatalyst material:
A) pure W18O49The preparation of photochemical catalyst: by 0.2gWCl6It is dissolved in 40mL dehydrated alcohol, and led into mixture
Enter 20mL polyethylene glycol (PEG), is vigorously stirred to after being completely dissolved and obtains photochemical catalyst presoma, the item for being 240 DEG C in temperature
Hydro-thermal process 20h obtains pure W under part18O49Photochemical catalyst sample (abbreviation W18O49)。
B) carbon quantum dot/W18O49The preparation of photocatalyst material sample: it is imported into above-mentioned photochemical catalyst presoma
After the carbon quantum dot ethanol solution prepared in 10mL embodiment step (2), hydro-thermal process under conditions of temperature is 240 DEG C
20h obtains carbon quantum dot/W18O49Photocatalyst material sample (abbreviation carbon quantum dot/W18O49)。
Performance test and analysis:
1) absorption property is tested
For the absorption property of the Pyrogentisinic Acid of analysis of material, prepared load carbon quantum dot/W is selected18O49Photocatalysis
Renewable porous carbon adsorbent, pure W18O49Photochemical catalyst, carbon quantum dot/W18O49Photocatalyst material, porous carbon adsorbent, point
Not Zuo Wei " adsorbent " to simulation phenolic waste water carry out absorption property test: 0.05g adsorbent, which is put into 50mL concentration, is
Mixture is obtained in the phenol solution of 500mg/L, pours into the beaker of 100mL and is placed in constant temperature blender with magnetic force, is existed respectively
A small amount of (equivalent) mixture filtering is taken when 0min, 30min, 60min, 90min, 120min, 150min, 180min, is taken after filtering
2mL solution is settled in 200mL volumetric flask, is measured using 4-AA direct spectrophotometry (HJ 503-2009)
Phenol in Aqueous Solution concentration.
2) regenerability is tested
For the Photocatalytic Regeneration performance of analysis of material, prepared load carbon quantum dot/W is selected18O49Photocatalysis can
Regenerate porous carbon adsorbent, pure W18O49Photochemical catalyst, carbon quantum dot/W18O49Four kinds of photocatalyst material, porous carbon adsorbent materials
Material, tests Photocatalytic Regeneration performance respectively as " adsorbent ": being by the concentration that 0.05g adsorbent puts into 50mL
It in the phenol solution of 500mg/L, is put into beaker and is placed in constant temperature blender with magnetic force, stir 30min absorption at room temperature
Pollutant, respectively in 0,15,30min by it is above-mentioned 1) in method survey Phenol in Aqueous Solution concentration, then by adsorbent and solution from
Adsorbent (solid isolated) after separation is put into glassware by heart separation, infrared with 200W at light source 20cm
Lamp irradiates 30min to adsorbent as near-infrared light source, after light-catalyzed reaction, is by the concentration that adsorbent rejoins 50mL
In the phenol solution of 500mg/L, adsorption experiment is repeated, is recycled 5 times repeatedly.
Interpretation of result:
Fig. 1 is that four contrast samples load carbon quantum dot/W in 180min18O49The renewable porous carbon adsorbent of photocatalysis,
Pure W18O49Photochemical catalyst, carbon quantum dot/W18O49The absorption of photocatalyst material, porous carbon adsorbent to 500mg/L phenol solution
Effect contrast figure.It can be seen from the figure that the sample prepared after being compounded with porous carbon materials is compared to pure W18O49Photocatalysis
The adsorption effect of Pyrogentisinic Acid has apparent promotion for agent, by carbon quantum dot and W18O49After compound, the Adsorption of Pyrogentisinic Acid
Efficiency is about 40%, it means that carbon material plays a very important role to the adsorption capacity tool of sample.Work as furfural wastewater with high concentration
By the porous carbon adsorbent and carbon quantum dot/W that carbonization generates after KOH is activated18O49It is right after photocatalyst material is compound
The removal rate of phenol greatly improves, and can achieve 80% or more.
The adsorption time of Fig. 2 sample is controlled in 30min, and every time after absorption, it is real that illumination sample 30min carries out regeneration
It tests, is then separated adsorbent from solution by the method for centrifugation.After drying, by sample carry out recycling and in this, as
Adsorbent carries out adsorption test again, and 5 times so on circulate, removal efficiency has respectively reached 65.3%, 62.7%,
64%, 61.9% and 60%.
It can be seen from the figure that sample is after 5 regeneration cycles, the removal efficiency of Pyrogentisinic Acid is still without excessively bright
Aobvious variation, absorption property lose within 6%, and removal efficiency still can be up to 60% or more in 30min.Show to load carbon amounts
Sub- point/W18O49The renewable porous carbon adsorbent of photocatalysis is stable during absorption and Photocatalytic Regeneration.It is possible thereby to
Conclusion out loads carbon quantum dot/W18O49The renewable porous carbon adsorbent of photocatalysis has extraordinary stability.
Fig. 3 is load carbon quantum dot/W18O49The SEM image of the renewable porous carbon adsorbent sample of photocatalysis, wherein scheming a
For photocatalysis regenerable sorbent low power figure, scheming b is adsorbent surface aperture high power figure.It can be seen from the figure that after by activating
Porous carbon formed hole in, carbon quantum dot/W18O49Photochemical catalyst is distributed in wherein, it was demonstrated that three compound successes of sample.
Fig. 4 is load carbon quantum dot/W18O49The transmission electron microscope picture of the renewable porous carbon adsorbent sample of photocatalysis is as schemed
Show.It can be seen from the figure that sample surfaces form after compound there are a large amount of pore channel in the sample of three-phase composite
Porous carbon chondritic.It irises out in arrow direction from figure it can be seen that carbon quantum dot/W18O49Photocatalyst material bead is high
Scheme as shown on the right again, and from the threadiness of bead surface it will also be seen that clearly lattice fringe, spacing of lattice are
0.23nm, with W18O49(511) crystal face characteristic peak of photochemical catalyst matches.Illustrate W18O49Photochemical catalyst successfully loads to
The surface of carbon quantum dot, and prove carbon quantum dot/W18O49Photocatalyst material has been successfully entered the hole of porous carbon materials sample
In road and combine.
Claims (10)
1. a kind of load carbon quantum dot/W18O49The preparation method of the renewable porous carbon adsorbent of photocatalysis, it is characterised in that: including
Following steps:
(1) preparation of porous carbon materials: furfural wastewater with high concentration carries out hydro-thermal reaction, filters to take solid, obtains precursor carbon material,
It with KOH aqueous solution soaking, dries, calcining obtains the porous carbon adsorbent using furfural wastewater with high concentration as carbon source；
(2) preparation of carbon quantum dot: citric acid mixes hydro-thermal reaction with urea, after being cooled to room temperature, uses syringe filter mistake
Filter, filtered filtrate dialysis, acquired solution freeze-drying obtain carbon quantum dot；Gained carbon quantum dot is dissolved in dehydrated alcohol, often
Carbon containing quantum dot 0.05g, obtains carbon quantum dot ethanol solution in 10mL solution；
(3) carbon quantum dot/W is loaded18O49The preparation of the renewable porous carbon adsorbent of photocatalysis: by WCl6It is dissolved in dehydrated alcohol
In, the porous carbon of polyethylene glycol, the carbon quantum dot ethanol solution of step (2) preparation and step (1) preparation is added into mixture
Adsorbent is added in pyroreaction kettle, hydro-thermal reaction after mixing, and gained mixture separation after reaction obtains load carbon amounts
Sub- point/W18O49The renewable porous carbon adsorbent of photocatalysis.
2. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (1) described furfural wastewater with high concentration, for the chaff under the primary distillation tower for the furfural for being 15% containing volume fraction
Aldehyde waste water.
3. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (1) described hydro-thermal reaction, reaction temperature is 200 DEG C, reaction time 8h.
4. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (1) described calcining, carries out under nitrogen protection, heating rate is 3 DEG C/min, calcination temperature 800
DEG C, the calcining at constant temperature time is 1h at 800 DEG C.
5. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: the mass ratio of step (2) citric acid and urea is 1:4.
6. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (2) described hydro-thermal reaction, reaction temperature is 160 DEG C, reaction time 6h；Reaction vessels are polytetrafluoro
Ethylene reaction kettle.
7. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (3) described WCl6Concentration in dehydrated alcohol is 0.005g/mL, the WCl6Quality and poly- second two
The ratio between volume of alcohol is 1:100g/mL, and the volume ratio of polyethylene glycol and carbon quantum dot ethanol solution is 2:1, porous carbon adsorbent
Quality and carbon quantum dot ethanol solution the ratio between volume 1:10g/mL.
8. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (3) described hydro-thermal reaction, reaction temperature is 240 DEG C, reaction time 20h.
9. load carbon quantum dot/W according to claim 118O49The preparation method of the renewable porous carbon adsorbent of photocatalysis,
It is characterized by: step (3) described separation, specifically: the centrifugation of gained mixture takes precipitating, and precipitating rinses weight with dehydrated alcohol
Centrifuging and taking precipitates and repeats this operation twice after outstanding, and gained is dried in vacuo under the conditions of precipitating 70 DEG C.
10. load carbon quantum dot/W according to claim 118O49The preparation side of the renewable porous carbon adsorbent of photocatalysis
Method, it is characterised in that: the concentration of step (1) the KOH aqueous solution is 1.12g/mL；Soaking time is 10-18h；Step (2) institute
Stating syringe filter filter sizes is 0.22 μm；Step (2) described dialysis, is dialysed using bag filter, through molecular weight 500-
100Da。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013664A (en) * | 2019-11-26 | 2020-04-17 | 燕山大学 | Composite photocatalyst and preparation method thereof |
| CN112103087A (en) * | 2020-09-17 | 2020-12-18 | 西北大学 | Method for preparing carbon quantum dot modified multistage tungsten trioxide-foamed nickel composite material and application thereof |
| CN112121842A (en) * | 2020-10-13 | 2020-12-25 | 南通职业大学 | Carbon nitride quantum dot/tungsten trioxide composite photocatalytic material and preparation method thereof |
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| CN113649048A (en) * | 2021-08-24 | 2021-11-16 | 青岛科技大学 | C-coated W5O14Quantum dot/C, N, O codoped MnxCd1-xS assembly and preparation method thereof |
| CN113649048B (en) * | 2021-08-24 | 2023-09-12 | 青岛科技大学 | C cladding W 5 O 14 Quantum dot/C, N, O co-doped Mn x Cd 1-x S assembly and preparation method thereof |
| CN116199224A (en) * | 2023-05-06 | 2023-06-02 | 成都达奇科技股份有限公司 | Preparation method of coal-based granular activated carbon, product and dye wastewater decoloring method |
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