CN110041016A - A kind of geo-polymer adsorbent material and preparation method thereof - Google Patents
A kind of geo-polymer adsorbent material and preparation method thereof Download PDFInfo
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- CN110041016A CN110041016A CN201910300343.2A CN201910300343A CN110041016A CN 110041016 A CN110041016 A CN 110041016A CN 201910300343 A CN201910300343 A CN 201910300343A CN 110041016 A CN110041016 A CN 110041016A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mineral polymers, e.g. geopolymers of the Davidovits type
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The present invention provides a kind of geo-polymer adsorbent material and preparation method thereof, the geo-polymer adsorbent material includes the following raw material in parts by weight: 15~35 parts of flyash, 65~85 parts of metakaolin, 40~120 parts of waterglass, 2~30 parts of sodium hydroxide and 30~90 parts of deionized water, preparation method is to be uniformly mixed each raw material to obtain injecting in mold after slurry, it carries out at 80 DEG C and under room temperature alternately conserving to get geo-polymer adsorbent material.The present invention is that low cost is prepared and with the geo-polymer adsorbent material of high absorption property in raw material using flyash and metakaolin etc., on the one hand new material is provided for removal heavy metal ions in sewage, on the other hand the resource utilization for realizing trade waste, has a good application prospect.
Description
Technical field
The present invention relates to adsorbent material fields more particularly to a kind of geo-polymer adsorbent material and preparation method thereof.
Background technique
Unprocessed be discharged into environment of industrial wastewater containing heavy metal can pollute soil and water body, to dynamic plant
The growth existence of object has an adverse effect.After heavy metal enters human body by food chain, eventually it is detrimental to health.Electricity
The industries such as plating, battery manufacture, printed circuit board and metal surface coating processing be generate containing heavy metal containing sewage it is important come
Source.
Currently, the method for heavy metal includes membrane separation technique, ion exchange technique, biologic treating technique, suction in purified water
Attached method and chemical precipitation etc..Absorption method is answered in sewage treatment extensively due to the features such as convenient, efficient and inexpensive
With.Traditional adsorbent material includes natural adsorbent material (such as zeolite, kaolin, diatomite, montmorillonite, wood fibre), people
Work adsorbent material (such as active carbon, carbon nanotube, nano fibrous membrane) and biological adsorption material (bacterium, fungi, algae etc.),
But these adsorbent materials still have the problems such as absorption property is poor, application cost is higher, to could not promote and apply on a large scale.
Geo-polymer is the inorganic polymer that aluminium silicate mineral powder and aqueous slkali are formed in 100 DEG C or less condensations,
With three dimensional polymeric structure and hole abundant.Geo-polymer durability, freeze thawing resistance, wearability and in terms of
Superior performance is shown, therefore is applied to building field and packing material in large quantities.In addition, geo-polymer also has height
It is also commonly used to solidify stable process field in toxic waste for the features such as intensity, acid and alkali-resistance and heat resistance.And utilize geology
Polymer is a new research field as the adsorbent of sewage treatment, the present invention is intended to provide a kind of absorption property it is good and at
This lower geology Polymer adsorption material.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of geo-polymer adsorbent material and preparation method thereof.
An object of the present disclosure is to provide a kind of geo-polymer adsorbent material, including following original in parts by weight
Material: 15~35 parts of flyash, 65~85 parts of metakaolin, 40~120 parts of waterglass, 2~30 parts of sodium hydroxide and deionized water
30~90 parts.
In above-mentioned technical proposal, using flyash, metakaolin, sodium hydroxide, waterglass and deionized water as raw material, pass through
Adjust each group distribution ratio, specially adjustment flyash and metakaolin ratio so as to adjust geo-polymer Si/Al ratio example,
The ratio of sodium hydroxide and waterglass is adjusted so as to adjust the Si/Na ratio of geo-polymer, inhales geo-polymer obtained
Enclosure material has preferable crushing resistance and biggish specific surface area, especially has and preferably adsorbs heavy metal energy.
Preferably, the geo-polymer adsorbent material includes the following raw material in parts by weight: flyash 30~35
Part, 65~75 parts of metakaolin, 60~70 parts of waterglass, 10~20 parts of sodium hydroxide and 30~50 parts of deionized water.
Preferably, the metakaolin is calcined 2~3h by kaolin raw ore powder at 800~1000 DEG C and is made.
It is made it is further preferred that the metakaolin calcines 3h by kaolin raw ore powder at 900 DEG C.
Preferably, the mesh number of the flyash and the metakaolin is not less than 100 mesh.
Preferably, the modulus of water glass is 1~4, further preferably 3.1~3.4.
Second purpose of the invention is to provide the preparation method of above-mentioned geo-polymer adsorbent material, and each raw material is mixed
It is injected in mold after uniformly obtaining slurry, carries out alternately conserving under the conditions of 80 DEG C and room temperature (15~35 DEG C) poly- to get geology
Close object adsorbent material.
Preferably, the preparation method specifically includes the following steps:
(1) flyash and metakaolin are uniformly mixed, obtain aluminosilicate powder；
(2) 10~30min of ultrasonic treatment is carried out after mixing waterglass and sodium hydroxide, then stands 12~48h, obtains alkali
Activator；
(3) aluminosilicate powder, the alkali activator and deionized water are mixed and stirred for, obtain geo-polymer
Homogenate；
(4) geo-polymer is homogenized after being sealed in injection mold, carries out at 80 DEG C and under room temperature alternately supporting
Shield, obtain geo-polymer block, then crushed, cross 30 meshes obtain geo-polymer adsorbent material.
Preferably, the actual conditions conserved in step (4) are as follows: 80 DEG C of air-proof condition conserve 12 hours --- air-proof condition room
Aeration condition room temperature is supported for temperature maintenance 12 hours --- 80 DEG C of air-proof condition maintenance 12 hours-air-proof condition room temperatures conserve 7 days ---
Shield 7 days.
Preferably, after geo-polymer block described in step (4) is crushed, is sieved, also progress deionized water washing
Air-dry, wash conditions are as follows: solid-liquid mass ratio 1:10, washing procedure are room temperature concussion washing 8 hours --- 90 DEG C of water-bath washings 5
Hour, wash 2 times --- it room temperature concussion washing 8 hours, washes 3 times.
As a kind of preferred embodiment of the present invention, the preparation method of geo-polymer adsorbent material the following steps are included:
(1) first prepare raw material in parts by weight: 30~35 parts of flyash, 65~75 parts of metakaolin, waterglass 60~
70 parts, 10~20 parts of sodium hydroxide and 30~50 parts of deionized water；
(2) flyash and metakaolin are uniformly mixed, obtain aluminosilicate powder；
(3) 10~30min of ultrasonic treatment is carried out after mixing waterglass and sodium hydroxide, then stands 12~48h, obtains alkali
Activator；
(4) aluminosilicate powder, the alkali activator and deionized water are mixed and stirred for, obtain geo-polymer
Homogenate；
(5) after the geo-polymer being homogenized injection mold sealing, conserved: 80 DEG C of air-proof condition maintenances 12 are small
When --- air-proof condition room temperature conserve 12 hours --- 80 DEG C of air-proof condition maintenance 12 hours-air-proof condition room temperatures conserve 7
It --- aeration condition room temperature conserve 7 days, obtain geo-polymer block, then crushed, cross 30 meshes obtain geology polymerization
Object adsorbent material.
Third purpose of the present invention be provide above-mentioned geo-polymer adsorbent material or preparation method in heavy metal adsorption, again
The application of metallic pollution processing and heavy metal recovery field.
The present invention is raw material using flyash and metakaolin etc., by adjusting each raw material proportioning and curing condition, preparation
Low cost and the geo-polymer adsorbent material with high absorption property are obtained, is on the one hand mentioned for removal heavy metal ions in sewage
For new material, on the other hand realizes the resource utilization of trade waste, have a good application prospect.Geology of the invention
Polymer adsorption material is to Pb in solution2+、Cd2+、Cu2+Saturated extent of adsorption distinguish 40.68~154.11mg/g, 30.56~
78.23mg/g and 11.64~36.61mg/kg.Preparation process of the present invention and appointed condition are simple, at low cost, are suitable for extensive raw
It produces.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is geo-polymer adsorbent material under the conditions of adsorption times different in the embodiment of the present invention 2 to Pb in solution2+'s
The variation diagram of adsorbance；
Fig. 2 is geo-polymer adsorbent material under the conditions of adsorption times different in the embodiment of the present invention 2 to Cd in solution2+'s
The variation diagram of adsorbance；
Fig. 3 is geo-polymer adsorbent material under the conditions of adsorption times different in the embodiment of the present invention 2 to Cu in solution2+'s
The variation diagram of adsorbance；
Fig. 4 is geo-polymer adsorbent material under the conditions of initial concentrations different in the embodiment of the present invention 3 to Pb in solution2+'s
The variation diagram of adsorbance and removal rate；
Fig. 5 is geo-polymer adsorbent material under the conditions of initial concentrations different in the embodiment of the present invention 3 to Cd in solution2+'s
The variation diagram of adsorbance and removal rate；
Fig. 6 is geo-polymer adsorbent material under the conditions of initial concentrations different in the embodiment of the present invention 3 to Cu in solution2+'s
The variation diagram of adsorbance and removal rate.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
The preparation of 1 geo-polymer adsorbent material of embodiment
The present embodiment provides a kind of geo-polymer adsorbent materials, including the following raw material in parts by weight: flyash
33.3 parts, 66.7 parts of metakaolin, 65.6 parts of waterglass, 14.4 parts of sodium hydroxide and 40 parts of deionized water；
Wherein, metakaolin is calcined 3h by kaolin raw ore powder at 900 DEG C and is made, flyash and metakaolin mistake respectively
100 meshes；Modulus of water glass is 3.3.
The preparation method of the geo-polymer adsorbent material of the present embodiment the following steps are included:
(1) flyash and metakaolin are uniformly mixed, obtain aluminosilicate powder；
(2) ultrasonic treatment 20min is carried out after mixing waterglass and sodium hydroxide, then is stood at room temperature for 24 hours, alkali is obtained
Activator；
(3) aluminosilicate powder of step (1), the alkali activator of step (2) and deionized water are mixed, and with 540r/
Min revolving speed stirs 30min, obtains geo-polymer homogenate；
(4) it by after the geo-polymer homogenate injection mold sealing of step (3), is conserved: 80 DEG C of air-proof condition maintenances
80 DEG C of air-proof condition maintenance 12 hours-air-proof condition room temperature maintenances 7 in 12 hours --- air-proof condition room temperature conserves 12 hours ---
It --- aeration condition room temperature conserve 7 days, obtain geo-polymer block, then crushed, cross 30 meshes obtain geology polymerization
Composition granule；
(5) the geo-polymer particle of step (4) is washed with deionized, solid-liquid mass ratio is 1:10 when washing, is washed
Washing program is room temperature concussion washing 8h --- 90 DEG C of water-bath washing 5h are washed 2 times --- room temperature concussion washing 8h, is washed 3 times, after air-drying
Up to target product geo-polymer adsorbent material.
Room temperature refers to 15~35 DEG C in above-mentioned preparation method.
Embodiment 2 using embodiment 1 geo-polymer adsorbent material under the conditions of different time in adsorbent solution a huge sum of money
Belong to ion
Utilize Pb (NO3)2、Cd(NO3)2With Cu (NO3)2Reagent prepares certain density heavy metal solution respectively, uses
NaOH and HNO3Adjust the pH of solution.Geo-polymer adsorbent material 0.1g is weighed, is added in 25ml heavy metal solution, 25
It is shaken under the conditions of DEG C, adsorbs heavy metal under the conditions of different time.It is 0.45 μm of filtering with microporous membrane adsorption liquid using aperture, leads to
Cross the concentration of Solution by Atomic Absorption Spectrophotometry heavy metal ion.
Wherein, each solution heavy metal ion initial concentration and initial pH are respectively as follows: Pb2+300mg/L, pH=3；Cd2+
300mg/L, pH=5；Cu2+200mg/L, pH=4.Adsorption time gradient is all provided with are as follows: 0,5,10,20,40,80,120,180,
240、300、400、600min。
Geo-polymer adsorbent material is to Pb in solution under the conditions of different adsorption times2+、Cd2+、Cu2+Adsorbance change
Change as shown in FIG. 1 to 3.It can be seen from the figure that geo-polymer adsorbent material is to Pb in solution2+、Cd2+、Cu2+Absorption reaches
Time to balance is respectively 240min, 300min and 240min, and equilibrium adsorption capacity is respectively 70.76,57.14 and 14.64mg/
g.Based on result above, the equilibration time of heavy metal in geo-polymer adsorbent material adsorbent solution can be set as 300min.
Embodiment 3 adsorbs the heavy metal of various concentration using the geo-polymer adsorbent material of embodiment 1
Utilize Pb (NO3)2、Cd(NO3)2、Cu(NO3)2Reagent prepares the heavy metal solution of various concentration gradient respectively, uses
NaOH and HNO3Adjust the pH of solution.Pb2+Initial pH be set as 3, initial concentration gradient is set as 100,200,300,500,800,
1000mg/L；Cd2+Initial pH be set as 5, initial concentration gradient is set as 50,100,200,300,500,800mg/L；Cu2+Just
Beginning pH is set as 4, and initial concentration gradient is set as 50,100,200,300,500mg/L.
Geo-polymer adsorbent material 0.1g is weighed, is added in 25ml heavy metal solution, is shaken under the conditions of 25 DEG C
300min makes absorption reach balance.It is 0.45 μm of filtering with microporous membrane adsorption liquid using aperture, it is molten by aas determination
The concentration of liquid heavy metal ion.
Geo-polymer adsorbent material is to Pb in solution under the conditions of different initial concentrations2+、Cd2+、Cu2+Adsorbance and go
Except the variation of rate is as shown in Fig. 4~Fig. 6.It can be seen from the figure that geo-polymer adsorbent material is to Pb2+、Cd2+、Cu2+Most
Big adsorbance can achieve 154.11,78.23 and 36.61mg/g respectively.Pb in solution2+Concentration be less than 500mg/L when, absorption
Material is to Pb2+Removal rate 91.57% or more；Cd in solution2+Concentration be less than 300mg/L when, adsorbent material is to Cd2+'s
Removal rate is 98.22% or more；Cu in solution2+Concentration be less than 100mg/L when, adsorbent material is to Cu2+Removal rate exist
95.17% or more.
Comparative example 1
It is maintenance processes with 1 difference of embodiment: geo-polymer slurry is conserved 14 days at room temperature.It obtains
Product easily becomes paste in water.
Comparative example 2
It is that aluminosilicate powder only contains flyash with 1 difference of embodiment.
Comparative example 3
It is that aluminosilicate powder only contains metakaolin with 1 difference of embodiment.
Comparative example 4
It is that aluminosilicate powder is metakaolin and zeolite, mass ratio 3:1 with 1 difference of embodiment；Its maintenance method
It sealed maintenance 24 hours under the conditions of being 50 DEG C, cools down, is then immersed in tap water in supporting under room temperature at room temperature
Shield 28 days.Curing time needed for this maintenance method is significantly larger than curing time of the invention.
Comparative example 5
The geo-polymer adsorbent material that this comparative example provides, including the following raw material in parts by weight: flyash 62
Part, 40 parts of metakaolin, 75 parts of waterglass, 33 parts of sodium hydroxide and 40 parts of deionized water, preparation method is the same as embodiment 1.
The geo-polymer adsorbent material of comparative example 2~5 carries out Pb according to the method in embodiment 32+、Cu2+、Cd2+Suction
Adhesion test examines each adsorbent material to the maximal absorptive capacity of heavy metal, and the results are shown in Table 1.
Maximal absorptive capacity of each geology Polymer adsorption material of table 1 to heavy metal
As can be seen from the above table, geo-polymer adsorbent material prepared by the present invention is to Pb2+、Cd2+And Cu2+Maximum inhale
Attached amount can achieve 154.11,78.23 and 36.61mg/g respectively, and the adsorbent material that comparative example is prepared is to Pb2+、Cd2+
And Cu2+Maximal absorptive capacity range be respectively 126.64~136.51mg/g, 52.82~69.47mg/g, 25.51~
30.94mg/g, adsorption capacity are obviously inferior to the geo-polymer adsorbent material that the present invention is prepared.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (9)
1. a kind of geo-polymer adsorbent material, which is characterized in that including the following raw material in parts by weight: flyash 15~
35 parts, 65~85 parts of metakaolin, 40~120 parts of waterglass, 2~30 parts of sodium hydroxide and 30~90 parts of deionized water.
2. a kind of geo-polymer adsorbent material according to claim 1, which is characterized in that including in parts by weight
The following raw material: it 30~35 parts of flyash, 65~75 parts of metakaolin, 60~70 parts of waterglass, 10~20 parts of sodium hydroxide and goes
30~50 parts of ionized water.
3. a kind of geo-polymer adsorbent material according to claim 1 or 2, which is characterized in that the metakaolin by
Kaolin raw ore powder is calcined 2~3h at 800~1000 DEG C and is made.
4. a kind of geo-polymer adsorbent material according to claim 3, which is characterized in that the metakaolin is by kaolinite
Native original ore powder is calcined 3h at 900 DEG C and is made.
5. a kind of geo-polymer adsorbent material according to claim 1 or 2, which is characterized in that the flyash and institute
The mesh number for stating metakaolin is not less than 100 mesh.
6. the preparation method of any one of Claims 1 to 5 geo-polymer adsorbent material, which is characterized in that will be described each
Raw material, which is uniformly mixed, to be obtained injecting in mold after slurry, at 80 DEG C and under room temperature alternately conserve and is polymerize to get geology
Object adsorbent material.
7. the preparation method of geo-polymer adsorbent material according to claim 6, which is characterized in that specifically include following
Step:
(1) flyash and metakaolin are uniformly mixed, obtain aluminosilicate powder；
(2) 10~30min of ultrasonic treatment is carried out after mixing waterglass and sodium hydroxide, then stands 12~48h, obtains alkali activation
Agent；
(3) aluminosilicate powder, the alkali activator and deionized water are mixed and stirred for, it is even obtains geo-polymer
Slurry；
(4) geo-polymer is homogenized after being sealed in injection mold, carries out at 80 DEG C and under room temperature replacing maintenance, obtains
To geo-polymer block, then crushed, cross 30 meshes obtain geo-polymer adsorbent material.
8. the preparation method of geo-polymer adsorbent material according to claim 7, which is characterized in that supported in step (4)
The actual conditions of shield are as follows: 80 DEG C of air-proof condition conserve 12 hours --- air-proof condition room temperature maintenance 12 hours --- air-proof condition 80
DEG C maintenance 12 hours-air-proof condition room temperature conserve 7 days --- aeration condition room temperature conserve 7 days.
9. the described in any item geo-polymer adsorbent materials of Claims 1 to 5 or the described in any item systems of claim 6~8
Preparation Method is in heavy metal adsorption, the application of heavy metal pollution processing and heavy metal recovery field.
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