CN106111060B - A kind of modification biological carbon composite and its preparation and application - Google Patents

A kind of modification biological carbon composite and its preparation and application Download PDF

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Publication number
CN106111060B
CN106111060B CN201610542090.6A CN201610542090A CN106111060B CN 106111060 B CN106111060 B CN 106111060B CN 201610542090 A CN201610542090 A CN 201610542090A CN 106111060 B CN106111060 B CN 106111060B
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China
Prior art keywords
carbon composite
biological carbon
modification biological
aluminum sulfate
sawdust
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CN201610542090.6A
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Chinese (zh)
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CN106111060A (en
Inventor
杨卫春
柴立元
周妍琦
刘礼彪
王海鹰
廖骐
唐崇俭
杨志辉
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中南大学
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • B01J20/08Solid 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 comprising aluminium oxide or hydroxide; comprising bauxite
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

Abstract

The invention discloses a kind of modification biological carbon composite and its preparations and application, include the following steps: aluminum sulfate solution sodium hydroxide solution adjusting pH to 5.0~7.0 boiling 5~30min of stirring, the sawdust that milled 140 mesh is added is mixed, it filters, freeze-day with constant temperature, it is carbonized to get modification biological carbon composite is arrived.The material preparation process is simple, easy to operate, low in cost, and physicochemical properties are stablized, good to the absorption property of Pb In Exhausted Water ion, without secondary pollution, and modification biological charcoal handles the lead waste water that initial concentration is 500mg/L, and adsorbance can reach 453.5mg/g.

Description

A kind of modification biological carbon composite and its preparation and application

Technical field

Modification biological carbon composite and preparation method thereof is prepared the present invention relates to a kind of utilization sawdust and Adsorption is useless The application of lead ion in water, belongs to biological carbon composite and its preparation and applied technical field.

Background technique

Chemical industry, metal smelt and processing process will generate a large amount of lead waste water, not reach without processing or processing such as It marks and is arbitrarily discharged into water body, it will cause water quality change dramatically, destroy water ecosystem;And it can pass through containing land pollutant Sediments and aquatile are enriched with, then are entered by food chain in the animal body of human body or other food chains high level and caused Lead poisoning.China's lead contamination at present is serious, and various regions " blood lead " event frequency is existing.

Absorption method is one of processing most important method of lead waste water, and the key of absorption method is the selection of adsorbent, often Adsorbent mainly includes activated alumina, ferriferous oxide, metal oxide, zeolite, active carbon etc..Charcoal has raw material The features such as source is wide, short texture is porous, surface-active function is more, physicochemical properties are stablized, in recent years, charcoal is in environment More and more paid attention to as water treatment absorbent in field.But charcoal surface group type is single, structure is uneven, The structures, functional defect such as hardly possible dispersion, limit it in the development in each field.

Timber is widely used in the industries such as pulp manufacture, earthwork, Furniture manufacture, and in the processing and manufacturing process of timber A large amount of sawdusts of middle generation are discarded mostly or are used as compost, recycled as low values such as the fuel recovery energy, from resource comprehensive For the angle utilized, this is the huge waste to biomass resource.And sawdust that is big using yield, making a low multiple use, The good modification biological carbon composite of large specific surface area, absorption property is prepared as adsorbent for giving up by the way that aluminum sulfate is modified The removal of lead ion in water, the high level for not only realizing sawdust recycle, and provide a kind of prepare for the processing of lead waste water New adsorbent at low cost, absorption property is strong, environmentally protective.

Summary of the invention

The present invention is intended to provide a kind of modification biological carbon composite and its methods for making and using same, the material preparation process Simply, production cost is low, high to the adsorption capacity of lead ion, without secondary pollution, is able to achieve the high-valued of sawdust biomass resource It utilizes.The processing application method that the modification biological carbon composite of preparation is applied to lead waste water is simple, and the time is short, operation side Just.

To achieve the above object of the invention, insight of the invention is that regulating and controlling to generate hydroxide by pH using aluminum sulfate solution Aluminium glue body and its sulfate ion, high sawdust is thoroughly mixed with phosphorus content, prepares modified biological carbon composite, can To change charcoal pore structure and improve charcoal specific surface area, and the functional group number of material surface can be significantly improved Amount increases the active site of lead ion absorption, to improve modification biological charcoal to the removal efficiency of Pb In Exhausted Water ion.

The purpose of the present invention is what is be accomplished by the following way.

A kind of preparation method of modification biological carbon composite, includes the following steps: aluminum sulfate solution sodium hydroxide Solution adjusts pH value, then boils stirring, and sawdust is ground, and is sieved, is added in the aluminum sulfate solution boiled, is sufficiently stirred, mistake Filter, it is dry, dry sample is carbonized, and logical protective gas protection, is kept the temperature after being warming up to final temperature, it is cooling, stop ventilation, then It cools down to get modification biological carbon composite is arrived.

The preparation method of the modification biological carbon composite, by 0.005~0.02mol/L aluminum sulfate solution hydrogen-oxygen Change sodium solution and adjusts pH value to 5.0~7.0.Stirring is boiled again boils 5~30min of stirring.Sawdust is ground, 140 meshes is crossed, adds Enter into the aluminum sulfate solution boiled.The aluminum sulfate solution volume and sawdust mass ratio are 50~1000mL/g.

The sawdust for grinding sieving, is added to the aluminum sulfate boiled by the preparation method of the modification biological carbon composite In solution, then magnetic agitation 30min is stirred 3~10 hours under room temperature, filter, and 60 DEG C of dryings 12 of thermostatic drying chamber are small When.The final temperature that is carbonized is 300~500 DEG C, and heating rate is 5 DEG C/min, and logical nitrogen protection, is warming up to after final temperature after keeping the temperature 1h, Stop ventilation, then cooled to room temperature when being cooled to 100 DEG C to get modification biological carbon composite is arrived.

The modification biological carbon composite is used to remove the lead ion in waste water.Specifically take the modification biological Carbon composite is added in the lead waste water of 20~500mg/L of plumbum ion concentration, according to modification biological carbon composite quality It is 0.1-1g.L-1 with wastewater volume ratio, under room temperature after oscillating reactions 5-720min, filtering.

Beneficial effects of the present invention:

(1) the present invention provides one kind using sawdust as raw material, the biological carbon composite of the modified preparation of aluminum sulfate, preparation side Method is simple, and production cost is low, and physicochemical properties are stablized, environmentally protective without secondary pollution, and industrial application prospect is high, use Sawdust source is wide, yield is big, make a low multiple use, it can be achieved that sawdust resource higher value application.

(2) material provided by the invention-modification biological carbon composite has very big specific surface area and higher hole Hold, material surface functional group is abundant, and adsorpting lead ion active site is more, can be matched by the retention of modification biological Carbon Materials, surface The effects of closing reaction, ion exchange realizes the efficient removal of Pb In Exhausted Water ion.

(3) modification biological Carbon Materials of the invention show the adsorption effect of lead compared to non-modified pure charcoal It writes and is promoted, adsorption capacity increases in several times.Modification biological charcoal handles plumbum ion concentration in 500mg/L or less, and adsorption capacity can Up to 453.5mg/g, and pure charcoal is only 96.2mg/g.

Detailed description of the invention

Fig. 1 is the transmission electron microscope picture of modification biological carbon composite in the embodiment of the present invention 1;

Fig. 2 is the transmission electron microscope picture without the modified pure biological carbon composite of aluminum sulfate;

Fig. 3 is nitrogen adsorption-desorption isotherm figure (a) of modification biological carbon composite and hole in the embodiment of the present invention 1 Diameter distribution map (b).

Specific embodiment

Illustrate that the present invention is described further below with specific embodiment, but it is necessary to note that following embodiment is only used In the further explanation to summary of the invention, limitation of the present invention not will form.

Embodiment 1

500mL0.01mol/L aluminum sulfate solution sodium hydroxide solution is adjusted into pH to 5.5, boils stirring 10min.It will Sawdust is ground with vibration sample grinding machine, and the sawdust 5g for taking 140 meshes to obtain is added in the aluminum sulfate solution boiled, magnetic agitation Then 30min is stirred 5 hours under room temperature, filter, 12 hours dry under the conditions of 60 DEG C of thermostatic drying chamber, by drying Sample carbonization, carbonization final temperature are 300 DEG C, and heating rate is 5 DEG C/min, and logical nitrogen protection, are warming up to after final temperature after keeping the temperature 1h, Stop ventilation, then cooled to room temperature when being cooled to 100 DEG C or so to get modification biological carbon composite is arrived.

Embodiment 2

500mL0.02mol/L aluminum sulfate solution sodium hydroxide solution is adjusted into pH to 6.0, boils stirring 10min.It will Sawdust is ground with vibration sample grinding machine, and the sawdust 5g for taking 140 meshes to obtain is added in the aluminum sulfate solution boiled, magnetic agitation Then 30min is stirred 5 hours under room temperature, filter, 12 hours dry under the conditions of 60 DEG C of thermostatic drying chamber, by drying Sample carbonization, carbonization final temperature are 400 DEG C, and heating rate is 5 DEG C/min, and logical nitrogen protection, are warming up to after final temperature after keeping the temperature 1h, Stop ventilation, then cooled to room temperature when being cooled to 100 DEG C or so to get modification biological carbon composite is arrived.

Embodiment 3

Under room temperature, with 0.02g embodiment 1 prepare material respectively to 20mL concentration be 80mg/L, 200mg/L and 500mg/L's carries out adsorption reaction containing lead solution, and wherein the reaction time is 6 hours, the plumbum ion concentration inductance coupling in filtrate Plasma emission spectrometer measurement is closed, lead ion adsorbance is respectively 76.3mg/g, 190.9mg/g and 453.5mg/g, removal Rate reaches 90% or more.

Embodiment 4

Under room temperature, with 0.02g embodiment 2 prepare material respectively to 20mL concentration be 40mg/L, 90mg/L, 200mg/L's and 300mg/L carries out adsorption reaction containing lead solution, and wherein the reaction time is 6 hours, the plumbum ion concentration in filtrate It is measured with inductive coupling plasma emission spectrograph, lead ion adsorbance is respectively 32.3mg/g, 73.5mg/g, 171.6mg/ G and 252.6mg/g.

Claims (9)

1. a kind of preparation method of modification biological carbon composite, which comprises the steps of: by 0.005 ~ 0.02 Mol/L aluminum sulfate solution sodium hydroxide solution adjusts pH value to 5.0 ~ 7.0;Stirring is boiled again, sawdust is ground, and is sieved, is added Enter into the aluminum sulfate solution boiled, be sufficiently stirred, filters, it is dry, dry sample is carbonized, and logical protective gas is protected Shield, keeps the temperature after being warming up to final temperature, cooling, stops ventilation, then cooling to get modification biological carbon composite is arrived.
2. the preparation method of modification biological carbon composite according to claim 1, which is characterized in that by aluminum sulfate solution After adjusting pH value with sodium hydroxide solution, then boil 5 ~ 30min of stirring.
3. the preparation method of modification biological carbon composite according to claim 1, which is characterized in that sawdust is ground, 140 meshes are crossed, are added in the aluminum sulfate solution boiled.
4. the preparation method of modification biological carbon composite according to claim 1, which is characterized in that the aluminum sulfate is molten Liquid is long-pending and sawdust mass ratio is 50 ~ 1000mL/g.
5. the preparation method of modification biological carbon composite according to claim 1, which is characterized in that sieving will be ground Sawdust is added in the aluminum sulfate solution boiled, magnetic agitation 30min, is then stirred 3 ~ 10 hours under room temperature, is filtered, permanent The drying 12 hours of 60 DEG C of warm drying box.
6. the preparation method of modification biological carbon composite according to claim 1, which is characterized in that carbonization final temperature be 300 ~ 500 DEG C, heating rate is 5 DEG C/min, and logical nitrogen protection, is warming up to after final temperature after keeping the temperature 1 h, when being cooled to 100 DEG C Stop ventilation, then cooled to room temperature to get modification biological carbon composite is arrived.
7. the modification biological carbon composite that method described in any one of claims 1-6 is prepared.
8. the application of modification biological carbon composite removal Pb In Exhausted Water ion as claimed in claim 7.
9. application according to claim 8, which is characterized in that take the modification biological carbon composite be added to lead from It is 0.1-1g/ according to modification biological carbon composite quality and wastewater volume ratio in the lead waste water of sub- 20 ~ 500 mg/L of concentration L, under room temperature after 720 min of oscillating reactions 5-, filtering.
CN201610542090.6A 2016-07-11 2016-07-11 A kind of modification biological carbon composite and its preparation and application CN106111060B (en)

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CN107056544A (en) * 2017-04-27 2017-08-18 河南农业大学 One kind promotes root growth high carbon-based soil remediation fertilizer and method
CN108585391B (en) * 2018-04-18 2019-07-05 中国海洋大学 A kind of charcoal renovation agent of the marine sediment of heavy metal pollution and preparation method thereof and restorative procedure

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