CN105413633B - It is a kind of suitable for heavy-metal adsorption material of high-calcium water-quality and preparation method and application - Google Patents
It is a kind of suitable for heavy-metal adsorption material of high-calcium water-quality and preparation method and application Download PDFInfo
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- CN105413633B CN105413633B CN201510968770.XA CN201510968770A CN105413633B CN 105413633 B CN105413633 B CN 105413633B CN 201510968770 A CN201510968770 A CN 201510968770A CN 105413633 B CN105413633 B CN 105413633B
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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
- C02F11/00—Treatment of sludge; Devices therefor
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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
- B01J2220/42—Materials comprising a mixture of inorganic materials
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The invention discloses a kind of suitable for heavy-metal adsorption material of high-calcium water-quality and preparation method and application.The heavy-metal adsorption material that the present invention is suitable for high-calcium water-quality is made of following pyrolysis substrates:Biophysics dewatered sludge and reduced iron powder;The mass ratio of the biophysics dewatered sludge and the reduced iron powder is 100~10:1.Its preparation method, includes the following steps:1) the biophysics dewatered sludge and the reduced iron powder are mixed, obtains the pyrolysis substrate;2) in an inert atmosphere, by the pyrolysis substrate pyrolysis;3) in the inert atmosphere, the pyrolysis substrate that will be handled through step 2) cools down, that is, obtains the heavy-metal adsorption material.Raw material of the present invention is cheap and easy to get, and can make municipal sludge recycling, avoids secondary pollution caused by municipal sludge;2nd, heavy metal absorbent of the present invention is in Ca2+In the higher water body of content, to the advantages of good adsorption effect of heavy metal ion, to the high treating effect of sewage.
Description
Technical field
The present invention relates to a kind of suitable for heavy-metal adsorption material of high-calcium water-quality and preparation method and application.
Background technology
Heavy metal persistently can be remained and accumulated in vivo, even if low dosage exposure can also seriously endanger ecological safety and
Health.Common heavy metal-polluted water purification techniques mainly has chemical precipitation, ion exchange, UF membrane etc., but these
There are the problems such as sludge yield is big, operating cost is high for technology.In contrast, absorption is superior technique selection, especially in water
When content of beary metal is relatively low in body.Activated carbon is most popular sorbing material, to reduce cost, finds the efficient of activated carbon
Cheaper alternative is the key of absorbing process.
China's municipal sludge yield is big, it is necessary to deals carefully with disposal, is just avoided that secondary pollution.After pyrolysis, in sludge
Organic matter transformation is the fuel gas such as tar and hydrogen, alkane, improves energy grade, is used easy to accumulating.Through biology-physics
Municipal sludge after drying and other treatment, particle is loose, more preferable beneficial to heat transfer, pyrolysis production capacity effect.Remaining solid residue after pyrolysis
For charcoal, further processing disposal or recycling are still needed to.Charcoal has the environmental functional similar with activated carbon, and nothing
Need to activate, cost is significantly less than activated carbon, can be as the repair materials of heavy metal-polluted water.
Ca in underground water and some polluted-waters2+Content is higher, can be competed with metal cation, so as to suppress adsorption material
Expect the repairing effect to heavy metal-polluted water.
The content of the invention
The object of the present invention is to provide it is a kind of suitable for heavy-metal adsorption material of high-calcium water-quality and preparation method thereof with should
With.Raw material of the present invention is cheap and easy to get, to the advantages of good adsorption effect of high calcium-containing Heavy Metals in Waters ion.
Heavy-metal adsorption material provided by the invention suitable for high-calcium water-quality, it is characterised in that:The heavy metal adsorption material
Material is made of following pyrolysis substrates:Biology-physics dewatered sludge and reduced iron powder;
The mass ratio of the biology-physics dewatered sludge and the reduced iron powder is 100~10:1.
In the present invention, the mass ratio of the biology-physics dewatered sludge and the reduced iron powder concretely 100:1、30:
1、15:1 or 10:1.
In above-mentioned heavy-metal adsorption material, the biology-physics dewatered sludge is according to including the following steps to prepare:By city
Political affairs sludge is through biology-physics drying and other treatment and air-dries obtained.
In above-mentioned heavy-metal adsorption material, the biology-physics drying and other treatment includes the following steps:The municipal administration is dirty
Mud and bark, which mix, to ferment to obtain the final product;
The time of the biology-physics drying and other treatment can be 7~15d, concretely 7d;
The dry basis ash content content of the biology-physics dewatered sludge can be 40%~60%, concretely 50%;
The quality moisture content of the biology-physics dewatered sludge can be 0~10%, concretely 2.24~2.42%;
During the specific biology-physics drying and other treatment, make the quality moisture content of the biology-physics dewatered sludge from 80%
Less than 50% is down to, moisture content further drops to less than 2.5% after air-drying.
In the present invention, the biology-physics drying and other treatment specifically comprises the following steps:By mass ratio 2:The 80% of 1 contains
Water rate municipal sludge and bark mix, and insert in vertical tubular composting tank (159L), and filling rate 75% is closed, top with
0.3m3/ h flows are evacuated draining;With 0.05m3/ hkgVS ventilation quantities make heap body heat up, and keep more than 65 DEG C 3~4d, add thereafter
Big ventilation quantity is to 3m3/ h is until processing terminates;
It is described air-dried to refer to spreading the sludge after biology-physics drying and other treatment in the shade ventilation to quality no longer
Change.
Present invention also offers the preparation method of above-mentioned heavy-metal adsorption material, include the following steps:1) by the life
Object-object manages dewatered sludge and reduced iron powder mixing, obtains the pyrolysis substrate;
2) in an inert atmosphere, by the pyrolysis substrate pyrolysis;
3) in the inert atmosphere, the pyrolysis substrate that will be handled through step 2) cools down, that is, obtains the heavy metal
Sorbing material.
In above-mentioned method, the inert atmosphere is nitrogen, carbon dioxide or helium;
The temperature of the pyrolysis can be 500~900 DEG C;
The time of the pyrolysis can be 15~120min.
In above-mentioned method, the temperature of the cooling can be 15~30 DEG C;
The time of the cooling can be 20~60min.
In above-mentioned method, the inert atmosphere can be nitrogen;
The temperature of the pyrolysis can be 900 DEG C;
The time of the pyrolysis can be 20min;
The temperature of the cooling can be 25 DEG C;
The time of the cooling can be 30min.
In above-mentioned method, the reaction unit of the pyrolysis is pyrolysis oven;The pyrolysis substrate can be placed in porcelain boat.
In the present invention, the particle diameter of the biology-physics dewatered sludge can be 0~0.45mm, concretely 0.45mm (i.e. 40
Mesh), specifically need to be molded in preparation process in commercial Application, grinding adjusts its particle diameter and can be omitted, the grain that can also be done
Footpath bigger.
Answering in heavy metal cation is removed in water body invention further provides above-mentioned heavy-metal adsorption material
With.
In above-mentioned application, the water body is calcic water body;
Calcium content is 20mg/L~2000mg/L in the water body;
The heavy metal sun is from at least one of cadmium ion, trivalent chromic ion, lead ion, zinc ion and copper ion.
The present invention has the following advantages:
1st, raw material of the present invention is cheap and easy to get, and can make municipal sludge recycling, avoids secondary pollution caused by municipal sludge;
2nd, heavy metal absorbent of the present invention is in Ca2+It is right to the advantages of good adsorption effect of heavy metal ion in the higher water body of content
The high treating effect of sewage.
Brief description of the drawings
Fig. 1 is heavy-metal adsorption material of the present invention in Cd2+-Ca2+To Cd in solution2+Adsorption effect.
Fig. 2 for heavy-metal adsorption material of the present invention in underground water to Cd2+Adsorption effect.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples, is commercially available unless otherwise specified.
Embodiment 1, suitable for high-calcium water-quality heavy-metal adsorption material preparation
Biology-physics dewatered sludge is municipal sludge (the specific mistake for handling and air-drying by biology-physics drying process
Journey is by mass ratio 2:1 80% moisture content municipal sludge is mixed with bark, is inserted in vertical tubular composting tank (159L), filling
Rate 75%, closed, top is with 0.3m3/ h flows are evacuated draining;With 0.05m3/ hkgVS ventilation quantities make heap body heat up, and keep 65
3~4d more than DEG C, thereafter stronger ventilation amount to 3m3/ h is until processing terminates;Then by the sludge after biology-physics drying and other treatment
Spread and no longer change in the shade ventilation to quality, screening recycling dewatered sludge.), dry basis ash content content about 50%.Municipal sludge
After biology-physics drying process processing, moisture content is down to less than 50%, and particle is loose, is easy to air-dried, moisture content after air-drying
2.33 ± 0.09%.
It is respectively 100 by biology-physics dewatered sludge and reduced iron powder mass ratio:1、30:1、15:1 and 10:1 formula
Substrate is prepared, according to following preparation methods:
1) substrate is sufficiently mixed, be placed in porcelain boat.
2) oxygen is caught up with to the greatest extent with nitrogen, porcelain boat is placed in pyrolysis oven, the lower 900 DEG C of reactions 20min of nitrogen atmosphere protection.
3) under nitrogen atmosphere protection, porcelain boat is released into heating zone, (about 25 DEG C) cooling 30min of room temperature.
4) remaining solid matter in porcelain boat is collected;Heavy-metal adsorption material of the present invention is obtained, is denoted as 1Fe respectively
BC900,3Fe@BC900,6Fe@BC900 and 10Fe@BC900.
Meanwhile by biology-physics dewatered sludge, pyrolysis prepares charcoal as stated above, BC900 is denoted as, as control
Group.Above-mentioned five kinds of sorbing materials are ground, it is spare to cross 40 mesh sieves (0.45mm).
Take each 50mg of above-mentioned 5 kinds of sorbing materials to be placed in 40mL glass sample bottles, be separately added into 25mL Cd2+-Ca2+It is molten
Liquid, is fully mixed, horizontal oscillations are stayed overnight at 25.0 ± 1.0 DEG C with whirlpool manufacture device.After adsorption equilibrium, filtered with 0.45 μm of polysulfones
Membrane filtration takes clear liquid, and remaining Cd in clear liquid is measured with ICP-OES methods2+Concentration.
Cd2+-Ca2+Solution is with Cd2+Stock solution and Ca2+Stock solution dilution is made, Cd2+Mass concentration about 200mg/L, Ca2+
Mass concentration scope is 0-200mg/L.Cd2+Stock solution is with Cd (NO3)2·4H2O, which is dissolved and diluted, is settled to mass concentration
2000mg/L is made.By 20mL concentrated nitric acids (substance withdrawl syndrome about 15mol/L) and 9.25g Ca (OH)2Mix, and dilute and determine
Hold the Ca for 500mL, obtaining 10000mg/L2+Stock solution.
In Cd2+-Ca2+In solution, heavy-metal adsorption material of the present invention is to Cd2+Adsorption effect it is as shown in Figure 1.Can by Fig. 1
Know, BC900 is to Cd2+Adsorption capacity with Ca2+Rise decrease, Ca2+Mass concentration 0mg/L when adsorption capacity
For 35.73 ± 1.30mg/g, Ca2+Mass concentration about 200mg/L when remain at 16.93 ± 0.20mg/g.Mix reduced iron
The sorbing material of powder is to Cd2+Adsorption effect it is more preferable, most preferably to account for biology-physics desiccation dirty for reduced iron powder quality for adsorption capacity
3Fe the@BC900, Ca of shale amount 3.33%2+Mass concentration 0mg/L when adsorption capacity be 64.56 ± 0.72mg/g, Ca2+
Mass concentration about 200mg/L when adsorption capacity be 31.42 ± 1.53mg/g.
Embodiment 2, suitable for high-calcium water-quality heavy-metal adsorption material preparation
3Fe@BC900 and BC900 are prepared according to preparation method in embodiment 1;Using activated carbon (being denoted as AC) and BC900 as pair
According to sorbing material.Above-mentioned three kinds of sorbing materials are ground, it is spare to cross 40 mesh sieves (0.45mm).
Prepared with underground water and contain Cd2+Solution.Taken Groundwater Property is as follows:Ca2+81.67mg/L、Mg2+38.95mg/L、
Na+25.42mg/L、K+1.87mg/L、NH4 +Do not detect, NO3 -21.06mg/L、Cl-34.88mg/L、SO4 2-70.76mg/L、
HCO3 -270.15mg/L、CO3 2-Do not detect.Cd2+Stock solution, by Cd (NO3)2·4H2O is dissolved with underground water, and enriching nitric acid is with ground
Lower water dilution is settled to 2000mg/L and (HNO is made30.2%).Experiment Cd2+Solution, concentration is with underground water dilution Cd on request2+
Stock solution is made.
The above-mentioned sorbing materials of 50mg are placed in 40mL glass sample bottles, add 25mL Cd2+-Ca2+Solution, with whirlpool system
Make device fully to mix, horizontal oscillations are stayed overnight at 25.0 ± 1.0 DEG C.After adsorption equilibrium, taken clearly with 0.45 μm of polysulfones membrane filtration
Liquid, remaining Cd in clear liquid is measured with ICP-OES methods2+Concentration.
Heavy-metal adsorption material of the present invention adsorbs Cd in underground water2+Effect it is as shown in Figure 2.As shown in Figure 2, AC pairs
Cd2+Adsorption capacity be no more than 25mg/g.The adsorption capacity of BC900 and sorbing material 3Fe@BC900 of the present invention will be significantly better than
AC, with Cd2+The increase of initial concentration and improve.Cd2+During initial concentration 185.49mg/L, BC900 and 3Fe@BC900 are to Cd2+
Adsorption capacity respectively reach 61.66 ± 0.41mg/g and 68.30 ± 3.11mg/g, 3Fe@BC900 are to Cd2+Adsorption capacity compared with
BC900 raisings more than 10% are AC to Cd2+4.32 times of adsorption capacity.
Claims (10)
- A kind of 1. heavy-metal adsorption material suitable for high-calcium water-quality, it is characterised in that:The heavy-metal adsorption material is by following heat Solution substrate is made:Biology-physics dewatered sludge and reduced iron powder;The mass ratio of the biology-physics dewatered sludge and the reduced iron powder is 100~10:1;The heavy-metal adsorption material is prepared according to the method included the following steps:1) biology-physics dewatered sludge and the reduced iron powder are mixed, obtains the pyrolysis substrate;2) in an inert atmosphere, by the pyrolysis substrate pyrolysis;3) in the inert atmosphere, the pyrolysis substrate that will be handled through step 2) cools down, that is, obtains the heavy metal adsorption Material;The temperature of the pyrolysis is 500~900 DEG C;The time of the pyrolysis is 15~120min.
- 2. heavy-metal adsorption material according to claim 1, it is characterised in that:The biology-physics dewatered sludge according to Include the following steps to prepare:Municipal sludge through biology-physics drying and other treatment and is air-dried obtained.
- 3. heavy-metal adsorption material according to claim 2, it is characterised in that:The biology-physics drying and other treatment includes Following steps:The municipal sludge and bark are mixed and fermented to obtain the final product;The time of the biology-physics drying and other treatment is 7~15d;The dry basis ash content content of the biology-physics dewatered sludge is 40~60%;The quality moisture content of the biology-physics dewatered sludge is 0~10%.
- 4. the preparation method of the heavy-metal adsorption material any one of claim 1-3, includes the following steps:1) by described in Biology-physics dewatered sludge and reduced iron powder mixing, obtain the pyrolysis substrate;2) in an inert atmosphere, by the pyrolysis substrate pyrolysis;3) in the inert atmosphere, the pyrolysis substrate that will be handled through step 2) cools down, that is, obtains the heavy metal adsorption Material.
- 5. according to the method described in claim 4, it is characterized in that:The inert atmosphere is nitrogen or helium;The temperature of the pyrolysis is 500~900 DEG C;The time of the pyrolysis is 15~120min.
- 6. method according to claim 4 or 5, it is characterised in that:The temperature of the cooling is 15~30 DEG C;The time of the cooling is 20~60min.
- 7. according to the method described in claim 6, it is characterised in that:The inert atmosphere is nitrogen;The temperature of the pyrolysis is 900 DEG C;The time of the pyrolysis is 20min;The temperature of the cooling is 25 DEG C;The time of the cooling is 30min.
- 8. method according to claim 4 or 5, it is characterised in that:The reaction unit of the pyrolysis is pyrolysis oven.
- 9. the heavy-metal adsorption material any one of claim 1-3 removes answering in heavy metal cation in water body With.
- 10. application according to claim 9, it is characterised in that:The water body is calcic water body;Calcium content is 20mg/L~2000mg/L in the water body;The heavy metal sun is from for cadmium ion, trivalent chromic ion, lead ion, zinc ion, copper ion.
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CN102167425A (en) * | 2011-03-23 | 2011-08-31 | 江苏陆博环保材料有限公司 | Method for preparing porous carbon-based compound micro electrolysis filter material |
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CN102167425A (en) * | 2011-03-23 | 2011-08-31 | 江苏陆博环保材料有限公司 | Method for preparing porous carbon-based compound micro electrolysis filter material |
CN103394333A (en) * | 2013-08-15 | 2013-11-20 | 北京航天益来电子科技有限公司 | Modified zeolite-fermented bark composite material, and preparation method and application thereof |
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