CN109550486A - A kind of preparation method of silica gel base weight metal absorbent - Google Patents

A kind of preparation method of silica gel base weight metal absorbent Download PDF

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CN109550486A
CN109550486A CN201910026085.3A CN201910026085A CN109550486A CN 109550486 A CN109550486 A CN 109550486A CN 201910026085 A CN201910026085 A CN 201910026085A CN 109550486 A CN109550486 A CN 109550486A
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silica gel
preparation
base weight
gel base
metal absorbent
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张海涛
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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
    • B01J20/046—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 containing halogens, e.g. halides
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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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Abstract

The invention discloses a kind of preparation method of silica gel base weight metal absorbent, include the following steps: prepared by (1) pretreatment of raw material and preparation, (2) raw material hybrid process, (3) finished product.The present invention has carried out special working process to adsorbent, improves the service performance of adsorbent, low adsorbent cost obtained well, it is easy to manufacture, and it uses stay in grade with very strong adsorption capacity, it is high-efficient, the great market competitiveness and application value.

Description

A kind of preparation method of silica gel base weight metal absorbent
Technical field
The invention belongs to silica gel processed and applied technical fields, and in particular to a kind of preparation side of silica gel base weight metal absorbent Method.
Background technique
Currently, with the development of industry, the industries such as metallurgy, plating, mine, chemical industry generate largely containing the waste water of heavy metal. More and more heavy metals enter in natural water body and soil, and do harm to huamn body.Heavy metal pollution of water body has become A big environmental problem urgently to be resolved in world wide.How to reduce and control heavy metal pollution is always world's environment protection field Hot issue.
Type, content and its existing forms of heavy metal ions in wastewater are different with different production types.It is currently used The method that removing heavy metals are removed from aqueous solution mainly include chemical precipitation method, hyperfiltration, absorption method, membrane separation process, Coagulation Method, Ion-exchange, electrochemical process etc..Wherein, absorption method is most effective and most widely used method.With other adsorbent material phases Than, active carbon and chelating resin using more and more extensive in Treatment of Industrial Water, but active carbon and business chelating resin material are high It is expensive, cost is too high.
Various adsorbents are prepared for this people exploitation, as application No. is a kind of shells disclosed in CN201510685850.4 Glycan-silica gel hybridization magnetic adsorbent and its preparation method and application carries out hydridization using chitosan and silica gel and suction has been made The attached dose of elimination to heavy metal, it is extensive with raw material sources, preparation process is simple, it is low in cost, can be recycled and ring The features such as border is friendly has reached the service performance of standard to the Adsorption effect of heavy metal.But as people are for product The continuous promotion that can be required, existing adsorbent still need to further enhance.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of preparation method of silica gel base weight metal absorbent is provided.
The present invention is achieved by the following technical solutions:
A kind of preparation method of silica gel base weight metal absorbent, includes the following steps:
(1) pretreatment of raw material and preparation:
A. chitosan and deionized water are put into agitator tank jointly according to 3 ~ 6:100 of weight ratio, it is poly- obtains shell after mixing Sugar juice is spare；
B. silica gel is put into incubator, adjusts the temperature in incubator to 110 ~ 115 DEG C, after 1 ~ 1.5h of isothermal holding it is living SiClx glue is spare；
C. by kaolin, corn fiber gum, waterglass, H2O2, deionized water it is corresponding according to 12 ~ 15:3 of weight ratio ~ 6:28 ~ 30:1 ~ 3:180 ~ 200 carry out mixing and put into agitator tank, are then stirred with 600 ~ 700 revs/min of revolving speed, 35 ~ 40min It is spare that mixed slurry A is obtained afterwards；
D. mixed slurry A made from operation c is slowly added dropwise in the beaker for filling polyglycol solution, then beaker is carried out Heating water bath, keeping bath temperature is 80 ~ 85 DEG C, is filtered after 3 ~ 4h of isothermal holding, then with deionized water to filtrate It is rinsed one time, it is spare that material B is finally obtained after being dried；
E. it will operate and cross 500 mesh after the resulting material B of d pulverizes, be then added into sodium alginate soln, while also to sea Nano-graphene is added in solution of sodium alginate, after magnetic agitation handles 1 ~ 2h, then chlorination is slowly added dropwise into sodium alginate soln Calcium solution is filtered after 14 ~ 16h of stewing process, dry that material C is spare after being rinsed one time with deionized water；
(2) raw material hybrid process:
A. following raw materials according: the resulting chitosan solution of 95 ~ 100 parts of step (1) operation a, 6 ~ 10 parts of steps is weighed by corresponding parts by weight Suddenly the resulting activated silica gel of (1) operation b, the resulting material C of 3 ~ 5 parts of step (1) operation e, 1 ~ 2 part of silane coupling agent；
B. will operate the weighed all raw materials of a put into reaction kettle jointly be stirred continuously 40 ~ 50min of processing after mixed liquor D It is spare；
(3) prepared by finished product:
By the resulting mixed liquor D of step (2) by droplet generator injection molding, deposition, aging process 2 ~ 3h system in lye At microballoon, later by microballoon from lye Magneto separate, then be washed with deionized one time, got product after drying process.
Further, kaolinic granular size described in step (1) operation c is 1 ~ 10 μm.
Further, the mass fraction of polyglycol solution described in step (1) operation d is 8 ~ 10%；The drying It is 75 ~ 80 DEG C that dry temperature is controlled when processing.
Further, the mass fraction of sodium alginate soln described in step (1) operation e is 2 ~ 4%, the nanometer The granular size of graphene is 10 ~ 50nm, and the amount that the material B is added is the 5 ~ 7% of sodium alginate soln gross mass, described The amount that is added of nano-graphene be the 3 ~ 5% of sodium alginate soln gross mass, the mass fraction of the calcium chloride solution is 7 ~ 9%。
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh550, silane coupling agent Any one in kh560, silane coupling agent kh570.
Further, the revolving speed of control stirring is 1200 ~ 1500 revs/min when stir process described in step (2) operation b Clock.
Further, lye described in step (3) is the sodium hydroxide solution that concentration is 2.5 ~ 3.5mol/L.
It further, is vacuum drying treatment when drying process described in step (3), during which the dry temperature of control is 60~65℃。
The present invention has carried out special Optimal improvements to adsorbent and has handled, still using chitosan, silica gel as bulk composition Processing preparation is carried out, ensure that the reduction of overall cost, in order to further improve its performance, also prepares and is added to a kind of object Expect C ingredient, this ingredient is a kind of recombination reaction object that adsorption reaction is very capable, is prepared in this forming process, first processing preparation Mixed slurry A is gone out, has been the slurries mixed using kaolin as matrix, has then carried out the preparation of material B, be by mixing slurry Expect that A carries out microsphere particle object made of balling-up solidification, finally carries out the processing of finished product materials C, be that material B is molten in sodium alginate React compound with nano-graphene, calcium chloride in liquid, a kind of gel ball obtained, the diameter of this gel ball is smaller, has fine Surface-active and adsorption reaction ability, when following process by the Compound Machinings such as this material C and chitosan solution, activated silica gel at Type embeds it in hybrid matrix, on the one hand can be crosslinked with activated silica gel etc., promote the stability of integral material, On the other hand it can also enhance whole adsorption capacity and efficiency, improve the adsorption effect to heavy metal etc..
The present invention has the advantage that compared with prior art
The present invention has carried out special working process to adsorbent, improves the service performance of adsorbent, suction obtained well Attached dose low in cost, easy to manufacture, and it is with very strong adsorption capacity, high-efficient using stay in grade, great market Competitiveness and application value.
Specific embodiment
Embodiment 1
A kind of preparation method of silica gel base weight metal absorbent, includes the following steps:
(1) pretreatment of raw material and preparation:
A. chitosan and deionized water are put into agitator tank jointly according to weight ratio 3:100, obtains chitosan after mixing Solution for standby；
B. silica gel is put into incubator, adjusts the temperature in incubator to 110 DEG C, after isothermal holding 1h activated silica gel is standby With；
C. by kaolin, corn fiber gum, waterglass, H2O2, deionized water is corresponding carries out according to weight ratio 12:3:28:1:180 Mixing is put into agitator tank, is then stirred with 600 revs/min of revolving speed, and it is spare that mixed slurry A is obtained after 35min；
D. mixed slurry A made from operation c is slowly added dropwise in the beaker for filling polyglycol solution, then beaker is carried out Heating water bath, keeping bath temperature is 80 DEG C, is filtered after isothermal holding 3h, is then rushed with deionized water to filtrate It washes one time, it is spare that material B is finally obtained after being dried；
E. it will operate and cross 500 mesh after the resulting material B of d pulverizes, be then added into sodium alginate soln, while also to sea Nano-graphene is added in solution of sodium alginate, after magnetic agitation handles 1h, then calcium chloride is slowly added dropwise into sodium alginate soln Solution is filtered after stewing process 14h, dry that material C is spare after being rinsed one time with deionized water；
(2) raw material hybrid process:
A. following raw materials according: the resulting chitosan solution of 95 parts of step (1) operation a, 6 parts of step (1) behaviour is weighed by corresponding parts by weight Make the resulting activated silica gel of b, the resulting material C of 3 parts of step (1) operation e, 1 part of silane coupling agent；
B. will operate the weighed all raw materials of a put into reaction kettle jointly be stirred continuously processing 40min after mixed liquor D it is standby With；
(3) prepared by finished product:
By the resulting mixed liquor D of step (2) by droplet generator injection molding, deposition, aging process 2h are made in lye Microballoon, later by microballoon from lye Magneto separate, then be washed with deionized one time, got product after drying process.
Further, kaolinic granular size described in step (1) operation c is 1 ~ 10 μm.
Further, the mass fraction of polyglycol solution described in step (1) operation d is 8%；At the drying It is 75 DEG C that dry temperature is controlled when reason.
Further, the mass fraction of sodium alginate soln described in step (1) operation e is 2%, the nanometer stone The granular size of black alkene is 10 ~ 50nm, and the amount that the material B is added is the 5% of sodium alginate soln gross mass, and described receives The amount that rice graphene is added is the 3% of sodium alginate soln gross mass, and the mass fraction of the calcium chloride solution is 7%.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh550.
Further, the revolving speed of control stirring is 1200 revs/min when stir process described in step (2) operation b.
Further, lye described in step (3) is the sodium hydroxide solution that concentration is 2.5mol/L.
It further, is vacuum drying treatment when drying process described in step (3), during which the dry temperature of control is 60℃。
Embodiment 2
A kind of preparation method of silica gel base weight metal absorbent, includes the following steps:
(1) pretreatment of raw material and preparation:
A. chitosan and deionized water are put into agitator tank jointly according to weight ratio 5:100, obtains chitosan after mixing Solution for standby；
B. silica gel is put into incubator, adjusts the temperature in incubator to 113 DEG C, after isothermal holding 1.2h activated silica gel It is spare；
C. by kaolin, corn fiber gum, waterglass, H2O2, deionized water is corresponding carries out according to weight ratio 14:5:29:2:190 Mixing is put into agitator tank, is then stirred with 650 revs/min of revolving speed, and it is spare that mixed slurry A is obtained after 38min；
D. mixed slurry A made from operation c is slowly added dropwise in the beaker for filling polyglycol solution, then beaker is carried out Heating water bath, keeping bath temperature is 82 DEG C, is filtered after isothermal holding 3.5h, is then carried out with deionized water to filtrate It rinses one time, it is spare that material B is finally obtained after being dried；
E. it will operate and cross 500 mesh after the resulting material B of d pulverizes, be then added into sodium alginate soln, while also to sea Nano-graphene is added in solution of sodium alginate, after magnetic agitation handles 1.6h, then chlorination is slowly added dropwise into sodium alginate soln Calcium solution is filtered after stewing process 15h, dry that material C is spare after being rinsed one time with deionized water；
(2) raw material hybrid process:
A. following raw materials according: the resulting chitosan solution of 98 parts of step (1) operation a, 8 parts of step (1) behaviour is weighed by corresponding parts by weight Make the resulting activated silica gel of b, the resulting material C of 4 parts of step (1) operation e, 1.5 parts of silane coupling agents；
B. will operate the weighed all raw materials of a put into reaction kettle jointly be stirred continuously processing 45min after mixed liquor D it is standby With；
(3) prepared by finished product:
By the resulting mixed liquor D of step (2) by droplet generator injection molding, deposition, aging process 2.5h system in lye At microballoon, later by microballoon from lye Magneto separate, then be washed with deionized one time, got product after drying process.
Further, kaolinic granular size described in step (1) operation c is 1 ~ 10 μm.
Further, the mass fraction of polyglycol solution described in step (1) operation d is 9%；At the drying It is 78 DEG C that dry temperature is controlled when reason.
Further, the mass fraction of sodium alginate soln described in step (1) operation e is 3%, the nanometer stone The granular size of black alkene is 10 ~ 50nm, and the amount that the material B is added is the 6% of sodium alginate soln gross mass, and described receives The amount that rice graphene is added is the 4% of sodium alginate soln gross mass, and the mass fraction of the calcium chloride solution is 8%.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh560.
Further, the revolving speed of control stirring is 1400 revs/min when stir process described in step (2) operation b.
Further, lye described in step (3) is the sodium hydroxide solution that concentration is 3.0mol/L.
It further, is vacuum drying treatment when drying process described in step (3), during which the dry temperature of control is 62℃。
Embodiment 3
A kind of preparation method of silica gel base weight metal absorbent, includes the following steps:
(1) pretreatment of raw material and preparation:
A. chitosan and deionized water are put into agitator tank jointly according to weight ratio 6:100, obtains chitosan after mixing Solution for standby；
B. silica gel is put into incubator, adjusts the temperature in incubator to 115 DEG C, after isothermal holding 1.5h activated silica gel It is spare；
C. by kaolin, corn fiber gum, waterglass, H2O2, deionized water is corresponding carries out according to weight ratio 15:6:20:3:200 Mixing is put into agitator tank, is then stirred with 700 revs/min of revolving speed, and it is spare that mixed slurry A is obtained after 40min；
D. mixed slurry A made from operation c is slowly added dropwise in the beaker for filling polyglycol solution, then beaker is carried out Heating water bath, keeping bath temperature is 85 DEG C, is filtered after isothermal holding 4h, is then rushed with deionized water to filtrate It washes one time, it is spare that material B is finally obtained after being dried；
E. it will operate and cross 500 mesh after the resulting material B of d pulverizes, be then added into sodium alginate soln, while also to sea Nano-graphene is added in solution of sodium alginate, after magnetic agitation handles 2h, then calcium chloride is slowly added dropwise into sodium alginate soln Solution is filtered after stewing process 16h, dry that material C is spare after being rinsed one time with deionized water；
(2) raw material hybrid process:
A. following raw materials according: the resulting chitosan solution of 100 parts of step (1) operation a, 10 parts of steps (1) is weighed by corresponding parts by weight Operate the resulting activated silica gel of b, the resulting material C of 5 parts of step (1) operation e, 2 parts of silane coupling agents；
B. will operate the weighed all raw materials of a put into reaction kettle jointly be stirred continuously processing 50min after mixed liquor D it is standby With；
(3) prepared by finished product:
By the resulting mixed liquor D of step (2) by droplet generator injection molding, deposition, aging process 3h are made in lye Microballoon, later by microballoon from lye Magneto separate, then be washed with deionized one time, got product after drying process.
Further, kaolinic granular size described in step (1) operation c is 1 ~ 10 μm.
Further, the mass fraction of polyglycol solution described in step (1) operation d is 10%；At the drying It is 80 DEG C that dry temperature is controlled when reason.
Further, the mass fraction of sodium alginate soln described in step (1) operation e is 4%, the nanometer stone The granular size of black alkene is 10 ~ 50nm, and the amount that the material B is added is the 7% of sodium alginate soln gross mass, and described receives The amount that rice graphene is added is the 5% of sodium alginate soln gross mass, and the mass fraction of the calcium chloride solution is 9%.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh570.
Further, the revolving speed of control stirring is 1500 revs/min when stir process described in step (2) operation b.
Further, lye described in step (3) is the sodium hydroxide solution that concentration is 3.5mol/L.
It further, is vacuum drying treatment when drying process described in step (3), during which the dry temperature of control is 65℃。
Comparative example 1
This comparative example 1 compared with Example 2, in step (1) pretreatment of raw material and preparation, is eliminated and is added in operation e Nano-graphene ingredient, method and step in addition to this is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, in step (2) raw material hybrid process, eliminates the step added in operation a Suddenly (1) operates the resulting material C ingredient of e, and method and step in addition to this is all the same.
Control group
Application No. is: a kind of chitosan-silica gel hybridization magnetic adsorbent disclosed in CN201510685850.4.
In order to compare effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, the corresponding system of control group The adsorbent obtained is tested for the property, and specific correlation data is as shown in table 1 below:
Table 1
Cu2+Eliminating rate of absorption (%) Zn2+Eliminating rate of absorption (%) Pb2+Eliminating rate of absorption (%) Ni2+Eliminating rate of absorption (%)
Embodiment 2 99.6 99.2 98.8 99.0
Comparative example 1 98.1 98.6 96.4 97.5
Comparative example 2 97.4 97.0 95.7 97.0
Control group 97.5 96.8 95.4 97.1
Note: Cu described in upper table 12+Eliminating rate of absorption, Zn2+Eliminating rate of absorption, Pb2+Eliminating rate of absorption, Ni2+Eliminating rate of absorption Experiment is to take 50ml containing Cu respectively2+ 10.0mg/L、Zn2+ 10.0mg/L、Pb2+ 10.0mg/L、Ni2+ 10.0mg/L laboratory Obtained aqueous solution, pH value are 5.5, are then respectively adding the corresponding adsorbent of 2.0g, then in 170 revs/min of revolving speed, temperature It under conditions of 25 DEG C, is placed in gas bath constant-temperature table and adsorbs 1h, take out adsorbent after absorption, then to more than after absorption Liquid measures Cu with atomic absorption spectrum respectively2+、Zn2+、Pb2+、Ni2+Concentration, and then calculate corresponding eliminating rate of absorption.
The adsorbent made from the method for the present invention it can be seen from upper table 1 is obviously improved the adsorption effect of heavy metal, pole Tool environmental protection, economic benefit are worth being widely applied.

Claims (8)

1. a kind of preparation method of silica gel base weight metal absorbent, which comprises the steps of:
(1) pretreatment of raw material and preparation:
A. chitosan and deionized water are put into agitator tank jointly according to 3 ~ 6:100 of weight ratio, it is poly- obtains shell after mixing Sugar juice is spare；
B. silica gel is put into incubator, adjusts the temperature in incubator to 110 ~ 115 DEG C, after 1 ~ 1.5h of isothermal holding it is living SiClx glue is spare；
C. by kaolin, corn fiber gum, waterglass, H2O2, deionized water it is corresponding according to 12 ~ 15:3 of weight ratio ~ 6:28 ~ 30:1 ~ 3:180 ~ 200 carry out mixing and put into agitator tank, are then stirred with 600 ~ 700 revs/min of revolving speed, after 35 ~ 40min It is spare to obtain mixed slurry A；
D. mixed slurry A made from operation c is slowly added dropwise in the beaker for filling polyglycol solution, then beaker is carried out Heating water bath, keeping bath temperature is 80 ~ 85 DEG C, is filtered after 3 ~ 4h of isothermal holding, then with deionized water to filtrate It is rinsed one time, it is spare that material B is finally obtained after being dried；
E. it will operate and cross 500 mesh after the resulting material B of d pulverizes, be then added into sodium alginate soln, while also to sea Nano-graphene is added in solution of sodium alginate, after magnetic agitation handles 1 ~ 2h, then chlorination is slowly added dropwise into sodium alginate soln Calcium solution is filtered after 14 ~ 16h of stewing process, dry that material C is spare after being rinsed one time with deionized water；
(2) raw material hybrid process:
A. following raw materials according: the resulting chitosan solution of 95 ~ 100 parts of step (1) operation a, 6 ~ 10 parts of steps is weighed by corresponding parts by weight Suddenly the resulting activated silica gel of (1) operation b, the resulting material C of 3 ~ 5 parts of step (1) operation e, 1 ~ 2 part of silane coupling agent；
B. will operate the weighed all raw materials of a put into reaction kettle jointly be stirred continuously 40 ~ 50min of processing after mixed liquor D It is spare；
(3) prepared by finished product:
By the resulting mixed liquor D of step (2) by droplet generator injection molding, deposition, aging process 2 ~ 3h system in lye At microballoon, later by microballoon from lye Magneto separate, then be washed with deionized one time, got product after drying process.
2. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (1) Operating kaolinic granular size described in c is 1 ~ 10 μm.
3. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (1) The mass fraction for operating polyglycol solution described in d is 8 ~ 10%；The dry temperature of control is 75 when the described drying process ~80℃。
4. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (1) The mass fraction for operating sodium alginate soln described in e is 2 ~ 4%, the granular size of the nano-graphene is 10 ~ 50nm, the amount that the material B is added is the 5 ~ 7% of sodium alginate soln gross mass, and the amount that the nano-graphene is added is The 3 ~ 5% of sodium alginate soln gross mass, the mass fraction of the calcium chloride solution are 7 ~ 9%.
5. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (2) Operating silane coupling agent described in a is silane coupling agent kh550, in silane coupling agent kh560, silane coupling agent kh570 Any one.
6. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (2) The revolving speed of control stirring is 1200 ~ 1500 revs/min when operating stir process described in b.
7. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (3) Described in lye be sodium hydroxide solution that concentration is 2.5 ~ 3.5mol/L.
8. a kind of preparation method of silica gel base weight metal absorbent according to claim 1, which is characterized in that step (3) Described in drying process when be vacuum drying treatment, during which the dry temperature of control is 60 ~ 65 DEG C.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111530434A (en) * 2020-05-13 2020-08-14 鲁东大学 Silica gel adsorbent for adsorbing heavy metal ions and preparation method thereof
CN115785646A (en) * 2022-11-25 2023-03-14 浙江月旭材料科技有限公司 Adsorption filler for purifying column and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111530434A (en) * 2020-05-13 2020-08-14 鲁东大学 Silica gel adsorbent for adsorbing heavy metal ions and preparation method thereof
CN115785646A (en) * 2022-11-25 2023-03-14 浙江月旭材料科技有限公司 Adsorption filler for purifying column and preparation method and application thereof

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