CN105056873B - A kind of preparation method of surface richness hydroxyl inorganic adsorbing material and application - Google Patents
A kind of preparation method of surface richness hydroxyl inorganic adsorbing material and application Download PDFInfo
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Abstract
A kind of preparation method of surface richness hydroxyl inorganic adsorbing material and application, are related to sorbing material.Method one:Oxide is subjected to first time baking after grinding, to drying after product of roasting hydration process, then is ground for the second time up to the surface richness hydroxyl inorganic adsorbing material.Method two:Oxide precursor is subjected to first time baking after grinding, drying after hydration process is carried out to product of roasting, then grind for the second time up to the surface richness hydroxyl inorganic adsorbing material.Method three:The mixture of oxide and oxide precursor is subjected to first time baking after grinding, drying after hydration process is carried out to product of roasting, then grind for the second time up to the surface richness hydroxyl inorganic adsorbing material.The surface richness hydroxyl inorganic adsorbing material can be applied in adsorbent containing heavy metal industrial effluent, nitrogenous and phosphorous industrial wastewater adsorbent, organic wastewater adsorbent is prepared.
Description
Technical field
The present invention relates to sorbing material, more particularly, to a kind of preparation method of surface richness hydroxyl inorganic adsorbing material with answering
With.
Background technology
The source of heavy metal wastewater thereby and widely distributed, is related to numerous industries such as mine, metallurgy, chemical industry, machinery, electronics.It is useless
The heavy metal being harmful in water includes lead, mercury, cadmium, zinc, chromium, copper, manganese etc..With the increase of all kinds of industry products, heavy metal contains
Amount and existing forms are also constantly occurring change.Waste water containing heavy metal ion directly discharges meeting in the case of without processing
Serious pollution is brought to surrounding enviroment.There is important show to China's economy and environment to waste water of the processing containing heavy metal ion
Sincere justice.
The method of existing heavy metal containing wastewater treatment can be substantially divided into three categories:(1) chemical method (the chemical agent precipitation method and
Electrolysis);(2) Physical (adsorbent such as activated carbon, ion exchange resin and membrane separation process);(3) bioanalysis.Gone in numerous
In the method for heavy metal pollution removing thing, heavy metal ion effectively adsorb so as to fulfill in water body using adsorbent
Heavy metals removal is a very promising approach, but existing adsorbent also has the problem of larger.For example, active raw material of wood-charcoal
Although expecting price inexpensively, its disposal ability is extremely limited, therefore using usually requiring to be modified before activated carbon adsorption, this is just
So that treatment process and cost rise;It is high although more notable using ion exchange resin or membrane separation process adsorption effect
Device requirement cause what it was greatly limited in the application.The quality decision of the Cost And Performance of adsorbent as can be seen here
It removes the effect of the heavy metal ion in polluted-water.
In recent years, nano-oxide (such as Fe is utilized2O3, Al2O3, MnO, TiO2Deng) surface charge and surface coordination etc. it is special
Property to the organic molecule in water body and heavy metal ion carry out absorption present good application prospect.Nano-oxide is usual
With high specific area, and its surface elecrtonegativity can have heavy metal ion preferable electrostatic adsorption in water body, receive at the same time
Rice oxide surface also possesses the hydroxyl being coordinated to heavy metal ion.What is more important, by controlling staying water
PH value, nano-oxide can exist relatively stablely in water body, will not be as hydrotalcite-like compound material in processing procedure
Material can be swapped out a large amount of metal ions when handling some heavy metal ion-containing waste waters, so as to cause secondary pollution.But nanometer
2 inherent shortcomings existing for oxide itself:1) particle diameter is small, and the colloidal sol separation of formation is difficult;2) surface can coordination site it is few,
Adsorption energy force difference.Therefore, this 2 inherent shortcomings of solution nano-oxide, can reduce the application cost of nano-oxide, at the same time
Lift its application prospect.
Chinese patent CN102266746A discloses a kind of preparation method of artificial synthesized inorganic crystal absorption material, by 10~
The prodan of 25wt%, the sodium carbonate of 2~20wt%, the silica of 30~60wt%, the magnesia of 15~45wt% mix
Close uniformly, which is fired into 6~20h by potcal pot calcination method or inner molten method at 600~1300 DEG C, obtains one kind
Molecular formula is Na (Mg2.5-0.5xNax) (Si4O10)F2The dilatancy artificial synthesized inorganic crystal absorption material of (0 < X≤1),
The material selectivity adsorption capacity is stronger, acid and alkali-resistance, high temperature resistant and radiation level higher, easy post-processing, is given birth in purified industrial
In terms of producing waste water, particularly in terms of radioactive nucleus waste water is handled, there is stronger practicality, and of low cost, production technology
Simply, have broad application prospects.
Chinese patent CN 103831080A disclose it is a kind of be used for recycle heavy metal ions in wastewater nickel slag sorbing material and
Its preparation method.This method is using industrial waste nickel slag and inexpensive analytical reagents aluminium hydroxide as primary raw material, through through raw material
After pretreatment, compressing, sintering and hydro-thermal process, the nickel slag sorbing material for heavy metal ions in wastewater absorption is made.
The sorbing material prepared through the method for the present invention has a series of excellent performance:Porosity is high, and specific surface area is big, to Pb2+、Cu2+
There is preferable absorption property etc. heavy metal ion;Further, since using molding method, the sorbent shapes of preparation, size
It is various, column, sheet, bulk etc. can be made, and with preferable intensity, it can be achieved that the regeneration cycle recycling profit of adsorbent
With.
The content of the invention
The purpose of the present invention is overcome the shortcomings of that existing nano-oxide during sewage containing heavy metal ion is handled, carries
Preparation method and application for a kind of surface richness hydroxyl inorganic adsorbing material.
One of the preparation method of the surface richness hydroxyl inorganic adsorbing material is as follows:
Oxide is subjected to first time baking after grinding, is to drying after product of roasting hydration process, then second of grinding
Obtain the surface richness hydroxyl inorganic adsorbing material.
The oxide may be selected from CaO and SiO2, and MgO, Fe3O4、Fe2O3、Al2O3It is at least one kind of in;The oxygen
Mass percent in compound between each component can be 55%~70%CaO, 10%~30%SiO2, 0~10%Fe2O3, 2%
~10%Al2O3, 0~5%MgO, total amount 100%, preferably 63.4%CaO, 24.4%SiO2, 4.9%Fe2O3, 7.3%
Al2O3。
The two of the preparation method of the surface richness hydroxyl inorganic adsorbing material are as follows:
Oxide precursor is subjected to first time baking after grinding, is dried after hydration process is carried out to product of roasting, then the
It is secondary to grind up to the surface richness hydroxyl inorganic adsorbing material.
The oxide precursor may be selected from Ca (OH)2、CaCO3、MgCO3、Mg(OH)2、Fe(OH)3、Al(OH)3、
Na2SiO3It is at least three kinds of in;Mass percent in the oxide precursor between each component is calculated by oxide form
Can be 55%~70%CaO, 10%~30%SiO2, 0~10%Fe2O3, 2%~10%Al2O3, 0~5%MgO, total amount is
100%.
The three of the preparation method of the surface richness hydroxyl inorganic adsorbing material are as follows:
The mixture of oxide and oxide precursor is subjected to first time baking after grinding, aquation is carried out to product of roasting
It is dry after processing, then grind for the second time up to the surface richness hydroxyl inorganic adsorbing material.
The oxide may be selected from CaO, MgO, SiO with oxide precursor mixture2、Fe3O4、Fe2O3、Al2O3、Ca
(OH)2、CaCO3、MgCO3、Mg(OH)2、Fe(OH)3Or Al (OH)3It is at least three kinds of in;The oxide and oxide precursor
It can be 55%~70%CaO, 10%~30% that mass percent in body mixture between each component is calculated by oxide form
SiO2, 0~10%Fe2O3, 2%~10%Al2O3, 0~5%MgO, total amount 100%.
At least 500 DEG C of the temperature of the roasting, the time at least 3min of the roasting;The temperature of the roasting preferably 800
~1500 DEG C, the time preferred 20min of the roasting.
The step of hydration process, is as follows:It is dispersed in water, stirs after product of roasting is cooled down.
The mass ratio of the water and product of roasting can be (20~5): 1, preferably 10: 1;The hydration treatment time period can be 8h
More than, preferably 12~24h.
The drying can use naturally dry or heat drying.
The time at least 1min, preferably 10~20min of the first time grinding.
The time at least 1min, preferably 10~20min of second of grinding.
The surface richness hydroxyl inorganic adsorbing material can be applied in adsorbent containing heavy metal industrial effluent is prepared, described to contain
Heavy metal industrial effluent can be that pH contains heavy metal industrial effluent, the heavy metal containing in heavy metal industrial effluent more than 3
Ion can be Cu2+、Ni2+、Cr3+、Fe3+、Hg2+At least one of Deng.
The surface richness hydroxyl inorganic adsorbing material can also be applied in nitrogenous and phosphorous industrial wastewater adsorbent is prepared.
The surface richness hydroxyl inorganic adsorbing material can also be applied in organic wastewater adsorbent is prepared.
Compared with prior art, the present invention has the advantages that following prominent:
(1) gained surface richness hydroxyl inorganic particle sorbing material has abundant surface hydroxyl, can be to the huge sum of money in water body
Belong to ion efficiently, quickly adsorb.
(2) compared with nano-oxide, richness hydroxyl inorganic particle sorbing material separation in gained surface is simple, by simple quiet
Put and can be carried out separating.
(3) gained surface richness hydroxyl inorganic particle sorbing material can also be to other pollutants such as organic matter in water body and ammonia nitrogen
There is removal ability, and have buffer capacity to acid waste water.
(4) ion friendship will not occur when handling effluent containing heavy metal ions for gained surface richness hydroxyl inorganic particle sorbing material
Phenomenon is changed, is not in secondary pollution.
(5) gained surface richness hydroxyl inorganic powder material is high to the adsorption capacity of heavy metal ion, processing is easy to operate.
(6) gained surface richness hydroxyl inorganic powder material processing heavy metal in water ion is of low cost, has good
Commercial Application prospect.
(7) preparation method of the surface richness hydroxyl inorganic powder material is of low cost, reaction unit is simple, preparation process
It is environmentally protective, reaction efficiency is high, post processing is simple.
Brief description of the drawings
Fig. 1 is infrared spectrum before and after 1 gained surface richness hydroxyl inorganic particle sorbing material hydration process of the embodiment of the present invention.
Embodiment
Below by embodiment combination attached drawing, the invention will be further described.
Embodiment 1
In a reservoir, by 3g CaCO3、0.8g SiO2、0.1g Fe2O3With 0.2g Al2O3Horse is positioned over after grinding 10min
1300 DEG C of roasting 15min are not warming up in stove, take a small amount of product of roasting to carry out infrared spectrum analysis, spectrogram is as shown in Figure 1;Roasting
(mass ratio of water and product of roasting is 5: 1) is dispersed in water after product cooling afterwards, after 12h is stirred at room temperature, filtering, filter cake
10min is ground after naturally dry in a reservoir up to required inorganic powder material, through infrared spectrum analysis, spectrogram as shown in Figure 1,
Wherein wave number about 3420cm-1Respective material surface hydroxyl, it can be seen that increase in aquation rear surface hydroxyl group, may infer that water
Adsorption efficiency higher after change.
Embodiment 2
In a reservoir, by 2.5g CaO, 0.5g SiO2、0.2g Fe2O3With 0.4g Al2O3Horse is positioned over after grinding 10min
1200 DEG C of roasting 15min are not warming up in stove, product of roasting is dispersed in water the (mass ratio of water and product of roasting after cooling
For 5: 1), after 24h is stirred at room temperature, filtering, filter cake grinds 10min up to required nothing after 60 DEG C of dryings in a reservoir in an oven
Machine powder body material.
2 gained surface richness hydroxyl inorganic powder material of the embodiment of the present invention is to nickel, copper, chromium (III) ion liquid waste processing side
Method is as follows:Alkali is added into ion waste liquid, adjusts the pH 3~6 of ion waste liquid, input quality is ion waste liquid 51 percent
Inorganic powder material, electromagnetic agitation 300rpm, stirs after 3h with 0.45 μm of membrane filtration, samples, sample inductive coupling
Plasma emission spectrometer (abbreviation ICP spectrometers) surveys its counter-ion concentrations.As can be seen from Table 1 in 3h, solution from
Sub- concentration can reach reduced levels, meet discharge standard,
Table 1 is 2 gained surface richness hydroxyl inorganic powder material of the embodiment of the present invention to Ni2+、Cu2+、Cr3+At ion waste liquid
Manage result.
Table 1
Embodiment 3
In a reservoir, by 2.8g CaCO3、0.8g Na2SiO3、0.3g Fe(OH)3With 0.4g Al2O3Grinding 10min is put
Put as 1200 DEG C of roasting 30min are warming up in Muffle furnace, product of roasting is dispersed in water (water and product of roasting after cooling
Mass ratio be 10: 1), after 24h is stirred at room temperature, filtering, filter cake grinds 10min after 60 DEG C of dryings in a reservoir in an oven
Up to required surface richness hydroxyl inorganic powder material.
The chemical nickel waste water of Electroplate Factory is handled with the inorganic powder material obtained by embodiment 3, contains higher COD in waste water
(400ppm or so), it is left containing the compounds such as copper, nickel, chromium, aluminium and total phosphorus (organophosphor and Phos) content 300ppm at the same time
It is right.
3 gained surface richness hydroxyl inorganic powder material of the embodiment of the present invention is as follows to chemical nickel method for treating waste liquid:Xiang Yi
Determine to put into the inorganic powder material that quality is waste liquid 5/1000ths in the chemical nickel waste water of volume, stand after rocking, used after 13h
0.45 μm of membrane filtration, sample, and sample surveys its each component equilibrium concentration with ICP spectrometers.Table 2 is the institute of the embodiment of the present invention 4
Inorganic powder material to chemical nickel wastewater treatment as a result, as can be seen from Table 2 in 13h, copper, nickel, chromium total content in solution
Reduced levels are can reach, total aluminium content is dropped to below discharge standard concentration, it is also seen that also having to phosphorus-containing compound certain
Removal ability.
Table 2
Embodiment 4
In a reservoir, by 3g Ca (OH)2、0.5g SiO2、0.4g Mg(OH)2With 0.4g Al2O3Grinding 10min place to
1100 DEG C of roasting 60min are warming up in Muffle furnace, product of roasting is dispersed in water the (matter of water and product of roasting after cooling
Amount is than being 10: 1), after 15h is stirred at room temperature, filtering, filter cake grinds 10min after 60 DEG C of dryings in a reservoir in an oven to obtain the final product
Required surface richness hydroxyl inorganic powder material.
Embodiment 5
In a reservoir, by 3g CaCO3、0.5g Na2SiO3、0.4g MgCO3With 0.4g Al (OH)310min is ground to place
As for 1300 DEG C of roasting 60min are warming up in Muffle furnace, product of roasting is dispersed in water to (water and product of roasting after cooling
Mass ratio is 20: 1), after 12h is stirred at room temperature, filtering, filter cake grinds 10min i.e. after 60 DEG C of dryings in a reservoir in an oven
Surface richness hydroxyl inorganic powder material needed for obtaining.
Embodiment 6
In a reservoir, by 6g CaCO3、2g Na2SiO3、1g Fe(OH)3With 1g Al (OH)3Grind 10min place as
1200 DEG C of roasting 30min are warming up in Muffle furnace, product of roasting is dispersed in water the (quality of water and product of roasting after cooling
Than for 10: 1), after 16h is stirred at room temperature, filtering, filter cake grinds 10min up to institute after 60 DEG C of dryings in a reservoir in an oven
Need surface richness hydroxyl inorganic powder material.
Embodiment 7
In a reservoir, by 4g CaCO3、1.5g Na2SiO3、0.5g Fe(OH)3With 1g Al (OH)3Put after grinding 10min
It is placed in Muffle furnace and is warming up to 1150 DEG C of roasting 40min, product of roasting is dispersed in water to (water and product of roasting after cooling
Mass ratio is 20: 1), after 8h is stirred at room temperature, filtering, filter cake grinds 10min after 60 DEG C of dryings in a reservoir in an oven to obtain the final product
Required surface richness hydroxyl inorganic powder material.
The present invention by being ground mixing, Ran Houjin in proportion by the oxide precursor mixture of Ca, Mg, Si, Mg, Fe
Row high-temperature calcination, then carries out aquation, filtering, drying and grinds up to surface richness hydroxyl inorganic adsorbing material.Synthetic method has
There is the features such as of low cost, reaction unit is simple, preparation process cleanliness without any pollution, reaction efficiency is high.Gained surface richness hydroxyl without
Machine sorbing material can be effectively treated single heavy metal ion in water body or contents of many kinds of heavy metal ion, while can be to water
The pollutant such as nitrogen, phosphorus and partial organic substances is handled in body.Surface richness hydroxyl inorganic adsorbing material will not in processing procedure
Generation secondary pollution.
Claims (15)
1. a kind of preparation method of surface richness hydroxyl inorganic adsorbing material, it is characterised in that it is comprised the following steps that:
Oxide is subjected to first time baking after grinding, to drying after product of roasting hydration process, then is ground for the second time up to institute
State surface richness hydroxyl inorganic adsorbing material;
The oxide is selected from CaO and SiO2, and MgO, Fe2O3、Al2O3In it is at least one kind of;
Mass percent in the oxide between each component is 55%~70%CaO, 10%~30%SiO2, 0~10%
Fe2O3, 2%~10%Al2O3, 0~5%MgO, total amount 100%.
A kind of 2. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 1, it is characterised in that the oxidation
Mass percent in thing between each component is 63.4%CaO, 24.4%SiO2, 4.9%Fe2O3, 7.3%Al2O3。
A kind of 3. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 1, it is characterised in that the roasting
At least 500 DEG C of temperature, the time at least 3min of the roasting.
A kind of 4. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 3, it is characterised in that the roasting
Temperature be 800~1500 DEG C, the time of the roasting is 20min.
A kind of 5. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 1, it is characterised in that the aquation
The step of processing, is as follows:It is dispersed in water, stirs after product of roasting is cooled down;
The mass ratio of the water and product of roasting is (20~5): 1, the hydration treatment time period is more than 8h;
The drying uses naturally dry or heat drying;
The time at least 1min of the first time grinding;
The time at least 1min of second of grinding.
A kind of 6. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 5, it is characterised in that the water with
The mass ratio of product of roasting is 10: 1;The hydration treatment time period is 12~24h;
The time of the first time grinding is 10~20min;
The time of second of grinding is 10~20min.
7. a kind of preparation method of surface richness hydroxyl inorganic adsorbing material, it is characterised in that it is comprised the following steps that:
Oxide precursor is subjected to first time baking after grinding, drying after hydration process, then second are carried out to product of roasting
Grind up to the surface richness hydroxyl inorganic adsorbing material;
The oxide precursor is selected from Ca (OH)2、CaCO3、MgCO3、Mg(OH)2、Fe(OH)3、Al(OH)3、Na2SiO3In
It is at least three kinds of;
Mass percent in the oxide precursor between each component by oxide form be calculated as 55%~70%CaO,
10%~30%SiO2, 0~10%Fe2O3, 2%~10%Al2O3, 0~5%MgO, total amount 100%.
A kind of 8. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 7, it is characterised in that the roasting
At least 500 DEG C of temperature, the time at least 3min of the roasting.
A kind of 9. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 7, it is characterised in that the aquation
The step of processing, is as follows:It is dispersed in water, stirs after product of roasting is cooled down;
The mass ratio of the water and product of roasting is (20~5): 1, the hydration treatment time period is more than 8h;
The drying uses naturally dry or heat drying;
The time at least 1min of the first time grinding;
The time at least 1min of second of grinding.
A kind of 10. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 9, it is characterised in that the roasting
800~1500 DEG C of temperature, the time 20min of the roasting;
The mass ratio of the water and product of roasting is 10: 1;The hydration treatment time period is 12~24h;
The time of the first time grinding is 10~20min;
The time of second of grinding is 10~20min.
11. a kind of preparation method of surface richness hydroxyl inorganic adsorbing material, it is characterised in that it is comprised the following steps that:
The mixture of oxide and oxide precursor is subjected to first time baking after grinding, hydration process is carried out to product of roasting
After dry, then grind for the second time up to the surface richness hydroxyl inorganic adsorbing material;The oxide is mixed with oxide precursor
Compound is selected from CaO, MgO, SiO2、Fe2O3、Al2O3、Ca(OH)2、CaCO3、MgCO3、Mg(OH)2、Fe(OH)3Or Al (OH)3In
It is at least three kinds of;
Mass percent in oxide and the oxide precursor mixture between each component is calculated as by oxide form
55%~70%CaO, 10%~30%SiO2, 0~10%Fe2O3, 2%~10%Al2O3, 0~5%MgO, total amount 100%.
A kind of 12. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 11, it is characterised in that the roasting
At least 500 DEG C of the temperature of burning, the time at least 3min of the roasting.
A kind of 13. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 11, it is characterised in that the water
The step of changing processing is as follows:It is dispersed in water, stirs after product of roasting is cooled down;
The mass ratio of the water and product of roasting is (20~5): 1, the hydration treatment time period is more than 8h;
The drying uses naturally dry or heat drying;
The time at least 1min of the first time grinding;
The time at least 1min of second of grinding.
A kind of 14. preparation method of surface richness hydroxyl inorganic adsorbing material as claimed in claim 13, it is characterised in that the roasting
The temperature of burning is 800~1500 DEG C, and the time of the roasting is 20min;
The mass ratio of the water and product of roasting is 10: 1;The hydration treatment time period is 12~24h;
The time of the first time grinding is 10~20min;
The time of second of grinding is 10~20min.
15. the surface richness hydroxyl inorganic adsorbing material as prepared by any the method for claim 1~14 contains heavy metal in preparation
Application in industrial wastewater adsorbent, nitrogenous and phosphorous industrial wastewater adsorbent, organic wastewater adsorbent;The work containing heavy metal
Industry waste water contains heavy metal industrial effluent for pH more than 3, and the heavy metal ion containing in heavy metal industrial effluent is Cu2+、Ni2 +、Cr3+、Fe3+、Hg2+At least one of.
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CN102190345A (en) * | 2010-03-10 | 2011-09-21 | 中国科学院福建物质结构研究所 | Method for enriching low-concentration heavy metal in water by recyclable magnesium hydroxide adsorbent |
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CN102190345A (en) * | 2010-03-10 | 2011-09-21 | 中国科学院福建物质结构研究所 | Method for enriching low-concentration heavy metal in water by recyclable magnesium hydroxide adsorbent |
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