CN110052239A - A kind of preparation method of dopen Nano magnesia compound bio charcoal - Google Patents
A kind of preparation method of dopen Nano magnesia compound bio charcoal Download PDFInfo
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- CN110052239A CN110052239A CN201910444335.5A CN201910444335A CN110052239A CN 110052239 A CN110052239 A CN 110052239A CN 201910444335 A CN201910444335 A CN 201910444335A CN 110052239 A CN110052239 A CN 110052239A
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- compound bio
- bio charcoal
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention discloses a kind of preparation method of dopen Nano magnesia compound bio charcoal, belongs to effluent containing heavy metal ions process field.The preparation method comprises the following steps: carboxymethyl cellulose is mixed with magnesium chloride soluble in water; heating volatilization moisture forms sticky glue; then it is instilled in ethanol solution; form fluffy hollow spheroidal particle; then it is pyrolyzed under nitrogen protection, has finally obtained the multiporous biological charcoal of dopen Nano magnesia.The compound bio charcoal has good removal effect to heavy metal ion such as copper, lead, cadmiums, and preparation method is simple, morphology controllable, low in cost.
Description
Technical field
The present invention designs a kind of preparation method and application technology of dopen Nano magnesia compound bio charcoal, belongs to industrial dirt
Water process range is specifically to handle the industrial wastewater containing heavy metal ion using the biological carbon, under conditions of pH > 2,
Can all have outstanding removal ability to various heavy metal ion.
Background technique
The factories such as plating, chemical industry, metal smelt in actual production can the heavy metals such as a large amount of cupric of output, lead, nickel from
Sub- waste water.And the main method of this kind of industrial wastewater is plus alkali neutralization sedimentation at present, but contained heavy metal in treated waste water
Ion concentration still reaches to also need further to handle less than discharge standard.
It is easily former with other with unsaturation due to lacking adjacent atom around nano magnesia particle surface atom
Son is combined and is settled out, thus has very strong adsorption capacity, and can reach adsorption equilibrium within a short period of time.But it receives
Rice grain recycling in distress, disadvantage easy to reunite, are restricted its application.The present invention has been obtained fluffy by sol-gel method
The compound bio charcoal precursor of pine, is evenly distributed in magnesium chloride on carboxymethyl cellulose surface, magnesium chloride meeting when pyrolysis
Uniform nano oxidized magnesium granules are formed, and releasing gas can make compound bio charcoal form porous structure, thus the compound life
In object Carbon Materials, nano magnesia and charcoal can play a role jointly, show quite outstanding go to heavy metal ion
Removing solid capacity.
A kind of Chinese invention patent " preparation method and application of water hyacinth-magnesia compound bio charcoal " (application number
201611114518.3) water hyacinth and magnesium oxide powder are uniformly mixed in, are then pyrolyzed to obtain mixture under nitrogen protection
To compound bio charcoal, a kind of patent " preparation method and application of magnesia-rice husk biology carbon composite " (application number
201611114669.9) by pyrolysis after rice husk charcoal and magnesia magma combination drying at compound bio charcoal in.But this
Compound bio charcoal prepared by two kinds of preparation methods has the deficiencies of magnesia doping is uneven, partial size is big, makes itself and nano oxygen
Change magnesium material compared to also with certain performance gap.Sol-gel method used in the present invention prepares compound bio charcoal precursor
Method have the advantages that be uniformly mixed, magnesia pattern it is regulatable, prepared dopen Nano magnesia by this method
Compound bio charcoal has many advantages, such as that adsorption capacity is big, the rate of adsorption is fast.
Summary of the invention
In order to overcome nano oxidized magnesium granules easy to reunite with charcoal to heavy metal ion adsorbed inefficient disadvantage, this hair
A kind of bright preparation method for being designed to provide dopen Nano magnesia compound bio charcoal based on sol-gel method, method
It is easy to operate, low in cost.
It is another object of the present invention to provide a kind of application of dopen Nano magnesia compound bio charcoal, institutes of the present invention
The adsorbent for stating method preparation can be used for the processing of heavy metal ion-containing waste water, have very outstanding go to ion of copper and lead
Removing solid capacity.
To achieve the above object, technical scheme is as follows:
A kind of preparation method of dopen Nano magnesia compound bio charcoal, the method are as follows:
(1) carboxymethyl cellulose and magnesium chloride are uniformly mixed according to certain mass ratio, are then dissolved in aqueous solution,
And solution is stirred evenly using mechanical stirring.
(2) after mixing evenly, heating heating is to vapor away moisture, when solution is sticky to one for the mixed solution in step (1)
It after determining degree, is added dropwise in ethanol solution using syringe, obtains fluffy hollow spheroidal particle.
(3) after the fluffy powder collection in step (2) being dried, under nitrogen protection using tube furnace, high temperature pyrolysis system
For at the charcoal with porous structure.
The mass ratio of carboxymethyl cellulose and magnesium chloride is 5:1-20:1 in the step (1), wherein carboxymethyl cellulose
Dose ratio with water is 1 g:50 mL-1 g:100 mL；The mechanical stirring time is 2-5 hours.
Temperature is 80-95 DEG C in the step (2)；Mixed liquor volume is concentrated to original 10 to ten/5th/
After one, at the uniform velocity it is added drop-wise in dehydrated alcohol dropwise using syringe.
Pyrolytical condition in the step (3) are as follows: the nitrogen protection in tube furnace, heating rate are 5-10 DEG C/min,
It is pyrolyzed 1-3 hours at 400-700 DEG C.
Beneficial effect
1. dopen Nano magnesia compound bio charcoal of the present invention is prepared using sol-gel method, magnesium ion is adsorbed
Cellulose afterwards can form porous fluffy precursor in ethanol, and the nano magnesia generated after pyrolysis is covered by multiporous biological
In charcoal, so that the material both has bigger serface, the absorption property of nano magnesia is also remained, thus to heavy metal ion
Have the characteristics that adsorption capacity is big, the rate of adsorption is fast.
2. the preparation method of dopen Nano magnesia compound bio charcoal of the present invention is simple, low in cost, and only
Using water and ethanol as solvent, there is no secondary pollution to environment.
3. can have quite outstanding removal effect under conditions of pH > 2 to effluent containing heavy metal ions, have wide in range
PH value use scope, compound bio Carbon Materials after absorption can directly aerobic pyrolysis generation metal oxide, reduce recycling
Pollution again in the process.
Detailed description of the invention
Fig. 1 is the flow diagram that the present invention prepares dopen Nano magnesia compound bio charcoal.
Fig. 2 is according to embodiments of the present invention 1, obtains the SEM figure of compound bio charcoal.
Fig. 3 is according to embodiments of the present invention 4, obtains compound bio charcoal absorption property with the relational graph of pH value of solution.
Specific embodiment
The contents of the present invention are described further combined with specific embodiments below, but the present invention be not limited solely to it is following
Embodiment, specific steps are referring to each embodiment.
Embodiment 1
(1) it takes 5 g carboxymethyl celluloses and 1 g magnesium chloride to be uniformly mixed respectively, is then dissolved in 500 mL aqueous solutions, and make
Solution is stirred evenly with mechanical stirring.
(2) mixed solution in step (1), using warming-in-water, is heated to 85 DEG C using after mechanical stirring 4 hours
Moisture is vapored away, when solution surplus is 200 mL, using syringe is dripped solution dropwise according to the speed of 5 mL/min
It is added in ethanol solution, wherein ethanol solution uses magnetic agitation, and the drop instilled in ethanol solution can quickly form fluffy
Hollow spheroidal particle.
(3) after the fluffy powder collection in step (2) being dried, under nitrogen protection using tube furnace, heating rate 10
DEG C/min, high temperature pyrolysis 2 hours at 500 DEG C are prepared into the charcoal with porous structure, the dry standby of secondary water washing
With.
Embodiment 2
(1) it takes 20 g carboxymethyl celluloses and 1 g magnesium chloride to be uniformly mixed respectively, is then dissolved in 2000 mL aqueous solutions, and
Solution is stirred evenly using mechanical stirring.
(2) mixed solution in step (1), using warming-in-water, is heated to 85 DEG C using after mechanical stirring 5 hours
Moisture is vapored away, when solution surplus is 300 mL, using syringe is dripped solution dropwise according to the speed of 5 mL/min
It is added in ethanol solution, wherein ethanol solution uses magnetic agitation, and the drop instilled in ethanol solution can quickly form fluffy
Hollow spheroidal particle.
(3) after the fluffy powder collection in step (2) being dried, under nitrogen protection using tube furnace, heating rate 10
DEG C/min, high temperature pyrolysis 2 hours at 400 DEG C are prepared into the charcoal with porous structure, the dry standby of secondary water washing
With.
Embodiment 3
The composite material is tested to the adsorption effect of practical copper-bearing industrial wastewater: obtaining the Industry Waste of copper ions from electroplate factory
Water contains a large amount of Na in the waste water+、Cl-、SO4 2-Solution is adjusted to pH=8 using sodium hydroxide, filtered out useless by plasma
Precipitating in water is 80 mg/L or so by the waste water copper ion concentration that Flame Atomic Absorption Spectrometry method is tested after preliminary treatment.Claim
It takes the compound bio charcoal prepared in 0.1 g embodiment 1 in conical flask, the waste water of 50 mL preliminary treatments, magnetic force is then added
After stirring 30 minutes, supernatant is taken to detect copper ions amount, discovery removal rate reaches 99.9% or more.Prove that the charcoal is multiple
Condensation material can remove copper ion from the industrial wastewater of system complexity.
Embodiment 4
The composite material is tested under different pH values to the adsorption effect of lead ion: the use of plumbi nitras configuration pH being 2,3,4,5,
6,7,8,9 concentration is the lead ion solution of 50 mg/L.The compound bio charcoal prepared in 0.1 g embodiment 1 is taken to be placed in conical flask
In, it is then respectively adding the lead nitrate solution of 50 mL difference pH, after magnetic agitation 30 minutes, supernatant is taken to use NITRATE BY FLAME ATOMIC
Absorption process detects lead ion surplus, and removal rate is as shown in Figure 3, it was demonstrated that the material in wider pH value range to lead ion all
With good removal ability.
Claims (4)
1. a kind of preparation method of dopen Nano magnesia compound bio charcoal, it is characterised in that: specific preparation process is as follows:
(1) carboxymethyl cellulose and magnesium chloride are uniformly mixed according to certain mass ratio, are then dissolved in aqueous solution, and make
Solution is stirred evenly with mechanical stirring；
(2) after mixing evenly, heating heating arrives certain journey to vapor away moisture, when solution is sticky to the mixed solution in step (1)
It after degree, is added dropwise in ethanol solution using syringe, obtains the hollow spheroidal particle of white；
(3) by after the fluffy powder collection drying in step (2), under nitrogen protection using tube furnace, high temperature pyrolysis is prepared into
Compound bio charcoal with porous structure.
2. the preparation method according to claim 1 for preparing dopen Nano magnesia compound bio charcoal, it is characterised in that: institute
Stating the mass ratio of carboxymethyl cellulose and magnesium chloride in step (1) is 5:1-20:1, wherein the dosage of carboxymethyl cellulose and water
Than for 1 g:50 mL-1 g:100 mL；The mechanical stirring time is 2-5 hours.
3. the preparation method according to claim 1 for preparing dopen Nano magnesia compound bio charcoal, it is characterised in that: institute
Stating temperature in step (2) is 80-95 DEG C；After mixed liquor volume is concentrated to original 1/5th, dripped dropwise using syringe
It is added in dehydrated alcohol.
4. the preparation method according to claim 1 for preparing dopen Nano magnesia compound bio charcoal, it is characterised in that: institute
State pyrolytical condition in step (3) are as follows: the nitrogen protection in tube furnace, heating rate is 5-10 DEG C/min, at 400-700 DEG C
Pyrolysis 1-3 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111871375A (en) * | 2020-08-17 | 2020-11-03 | 常州大学 | Preparation method and application of biochar with efficient atrazine adsorption performance |
| CN112108118A (en) * | 2020-09-21 | 2020-12-22 | 黄河水利职业技术学院 | Magnetic biomass charcoal based on Fenton sludge and cellulose and preparation method and application thereof |
| CN112156756A (en) * | 2020-10-12 | 2021-01-01 | 浙江农林大学 | Corn straw carbon-based nano adsorbent and preparation method thereof |
| CN113087065A (en) * | 2021-05-06 | 2021-07-09 | 哈尔滨工业大学 | Method for improving lead ion removal capability of adsorbent by using carbon dioxide |
| CN115672276A (en) * | 2022-12-26 | 2023-02-03 | 昆明理工大学 | Method for enhancing copper ion adsorption of biochar by utilizing magnesium chloride modification |
| CN117531475A (en) * | 2023-10-27 | 2024-02-09 | 中国热带农业科学院橡胶研究所 | Magnesia doped nano magnesium hydroxide loaded biochar and preparation method and application thereof |
| CN117531475B (en) * | 2023-10-27 | 2024-05-31 | 中国热带农业科学院橡胶研究所 | Magnesia doped nano magnesium hydroxide loaded biochar and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111871375A (en) * | 2020-08-17 | 2020-11-03 | 常州大学 | Preparation method and application of biochar with efficient atrazine adsorption performance |
| CN112108118A (en) * | 2020-09-21 | 2020-12-22 | 黄河水利职业技术学院 | Magnetic biomass charcoal based on Fenton sludge and cellulose and preparation method and application thereof |
| CN112156756A (en) * | 2020-10-12 | 2021-01-01 | 浙江农林大学 | Corn straw carbon-based nano adsorbent and preparation method thereof |
| CN113087065A (en) * | 2021-05-06 | 2021-07-09 | 哈尔滨工业大学 | Method for improving lead ion removal capability of adsorbent by using carbon dioxide |
| CN115672276A (en) * | 2022-12-26 | 2023-02-03 | 昆明理工大学 | Method for enhancing copper ion adsorption of biochar by utilizing magnesium chloride modification |
| CN117531475A (en) * | 2023-10-27 | 2024-02-09 | 中国热带农业科学院橡胶研究所 | Magnesia doped nano magnesium hydroxide loaded biochar and preparation method and application thereof |
| CN117531475B (en) * | 2023-10-27 | 2024-05-31 | 中国热带农业科学院橡胶研究所 | Magnesia doped nano magnesium hydroxide loaded biochar and preparation method and application thereof |
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