CN110449142A - A kind of magnetic silica porous adsorbent and its preparation method and application - Google Patents
A kind of magnetic silica porous adsorbent and its preparation method and application Download PDFInfo
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- CN110449142A CN110449142A CN201910701960.3A CN201910701960A CN110449142A CN 110449142 A CN110449142 A CN 110449142A CN 201910701960 A CN201910701960 A CN 201910701960A CN 110449142 A CN110449142 A CN 110449142A
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
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Abstract
The invention discloses a kind of magnetic silica porous adsorbents and its preparation method and application.The preparation of magnetic silica porous adsorbent includes the following steps: to mix SiO 2 powder and ferric ion solutions, 60~80 DEG C of hot alkaline solution is added, pH is adjusted, is sufficiently down to room temperature ageing, washing to neutrality after reaction, drying and grinding obtains magnetic silica porous adsorbent.The preparation method of magnetic silica porous adsorbent of the invention, using inorganic silicon source SiO 2 powder as raw material, it is not only cheap and easy to get, and asepsis environment-protecting, it is generated in preparation process without related organic liquid waste, it is environmental-friendly, using with surface deposition, cryogenic conditions synthesize in next step, and the reaction time is short, preparation process less energy consumption, it is at low cost.Magnetic silica porous adsorbent has good selectivity, and the maximal absorptive capacity to methylene blue is 121.23mg/g, to the maximal absorptive capacity 163.52mg/g of malachite green.
Description
Technical field
The present invention relates to techniques of Dyeing Wastewater Treatment fields, more particularly, to a kind of porous absorption of magnetic silica
Agent and its preparation method and application.
Background technique
To water pollution control, more stringent requirements are proposed for the promulgation of " ten, water ", and industrial wastewater is as difficult to deal with one
Class waste water is constantly subjected to pay close attention to, and dyeing waste water is the higher a kind of waste water of accounting in industrial wastewater discharge total amount, printing and dyeing
Waste water organic concentrations are high, and coloration is big, and chemical property is stablized, difficult biochemical, are a kind of industrial wastewaters that processing difficulty is big.Printing and dyeing are useless
Water is after Physiochemical and biochemical is handled, and wherein pollution index substantially reduces, and can largely reach discharge standard, but as standard is arranged
The raising put, current processing method technology realize that this target is increasingly difficult to.Absorption method is in numerous technologies because of operation letter
Single, at low cost, high-efficient to be favored, in absorption method, the selection of adsorbent material is the most key, therefore selects one kind
Efficiently, selectivity is good, and inexpensive adsorbent material is to determine to adsorb successful deciding factor.Magnetic material has magnetic strong, easy
The advantages that separating, be reusable, but magnetic material adsorption effect and adsorptive selectivity are poor.Silica is wide on earth
It is general there is, inexpensive easily to take, and silica acid and alkali-resistance, stability is high, by silica and magnetic material it is compound be absorption
The hot spot in investigation of materials field.The some new methods for preparing magnetic silica composite material developed in recent years have template,
Sol-gal process, reverse microemulsion process etc., the preparation of these methods is more many and diverse, and the time is long and can all use certain organic molten
Agent, this may bring secondary pollution to environment.For example, CN107583599A discloses a kind of monodisperse mesoporous silica
Preparation, application and the regeneration method of adsorbent are reacted and post-treated obtain single point by CTAB, THEED and TEOS
Mesoporous silicon oxide adsorbent is dissipated, the addition of organic substance causes the discharge of organic liquid waste in preparation process, forms secondary dirt
Dye.This field is it is contemplated that a kind of environmental-friendly be easily-synthesized and the preparation of the silica magnetic adsorbent material of efficient absorption
Method.
Summary of the invention
The technical problem to be solved by the present invention is to overcome existing silica magnetic adsorbent material preparation process to be easy to produce
It is porous to provide a kind of magnetic silica for secondary pollution, adsorption treatment poor selectivity, adsorption efficiency not high defect and deficiency
The preparation method of adsorbent.
Another object of the present invention is to provide the magnetic silica porous adsorbents that the above method is prepared.
Another object of the present invention is to provide a kind of magnetic silica porous adsorbents in dyeing waste water adsorption treatment
In application.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps: SiO 2 powder and iron
Solion mixing, is added 60~80 DEG C of hot alkaline solution, adjusts pH to 10.00~12.00, and it is old to be down to room temperature after point reaction
Change washing to neutrality, drying and grinding obtains magnetic silica porous adsorbent,
Wherein ferric iron and ferrous molar ratio are 1.8~2.0:1, SiO 2 powder and three in ferric ion solutions
The molar ratio of valence iron is 1~3:1, and reaction temperature is 60~80 DEG C, 60~120min of reaction time.
PH value range and reaction temperature of the invention not only influences the generation of reaction, has an effect on reaction and speed occurs.
The present invention using SiO 2 powder as preparation raw material, be as inorganic silicon source SiO 2 powder it is nontoxic,
Raw material that is cheap and being easy acquisition.The present invention uses surface deposition, single step reaction, that is, synthesizing magnetic porous silica simultaneously
High-efficiency adsorbent, without reference to organic solvent in reaction process, reaction process carries out at low temperature, and the reaction time is short, preparation
Process less energy consumption, advantage at low cost and environmentally friendly.Meanwhile magnetic silica porous high-efficiency adsorbent tool prepared by the present invention
It is magnetic, can be quickly separated by solid-liquid separation using magnetic field, the material after adsorbing dyestuff can use the acid desorption of low concentration, repeat
Utilization rate is high.
It is wherein preferably added to thermokalite and ferric molar ratio is 8~9:1.
Preferably, the SiO 2 powder and ferric molar ratio are 2~3:1.
Preferably, the pH is adjusted to 11~12.
It is highly preferred that the ferric iron and ferrous molar ratio are 1.8:1, SiO 2 powder rubs with ferric
, than being adjusted to 11 for 2:1, pH, reaction temperature is 60 DEG C for you.
It is same it is highly preferred that the ferric iron and ferrous molar ratio are 2:1, SiO 2 powder with it is ferric
Molar ratio is 3:1, and pH is adjusted to 12, and reaction temperature is 80 DEG C.
Preferably, the digestion time is 1~3h.Preferably 1h.
The magnetic silica porous adsorbent that the present invention also protects the preparation method to be prepared.
Application of the magnetic silica porous adsorbent in the Adsorption dyeing waste water dye of positive ion is also at this
Within the protection scope of invention.
The dye of positive ion of the preferred Adsorption of magnetic silica porous adsorbent is methylene blue and malachite
It is green.
Compared with prior art, the beneficial effects of the present invention are:
(1) the present invention provides a kind of preparation methods of magnetic silica porous adsorbent, using inorganic silicon source dioxy
SiClx powder is not only cheap and easy to get as raw material, and asepsis environment-protecting, generates in preparation process without related organic liquid waste, environment friend
It is good；
(2) preparation method of magnetic silica porous adsorbent of the invention, which uses, uses surface deposition, cryogenic conditions
It synthesizes in next step, the reaction time is short, preparation process less energy consumption, at low cost；
(3) magnetic silica porous adsorbent of the invention has good selectivity, to the dye of positive ion have compared with
High adsorption capacity, the maximal absorptive capacity to methylene blue is 121.23mg/g, to the maximal absorptive capacity of malachite green
163.52mg/g。
Specific embodiment
The present invention is further illustrated With reference to embodiment, but embodiment does not appoint the present invention
The restriction of what form.Unless otherwise indicated, source chemicals used in the embodiment of the present invention are the source chemicals routinely bought.
Embodiment 1
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) 2.00g (0.005mol) Fe is weighed respectively2(SO4)3, 1.20g (0.02mol) SiO 2 powder and 1.40g
(0.005mol)FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:SiO2=2:1:4.First by Fe2(SO4)3And silica
Powder is added in 100ml deionized water, ultrasonic disperse 10min, then magnetic agitation, to being completely dissolved, whipping temp is 60 DEG C, so
Afterwards plus FeSO4·7H2O stirring a few minutes make ferrous ion be completely dissolved to obtain mixed solution.
(2) sodium hydroxide 1.60g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring adjusts pH to 11, and temperature is controlled at 60 DEG C, reacted 120 minutes by heating, stops heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying is ground after 12 hours up to Fe in a vacuum drying oven3+:SiO2The magnetic of=1:2
Property porous silica high-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 1
Ionic dye waste water measures its absorption property to dyestuff.Prepare the simulated wastewater that dye solution is 10~100mg/L, waste water
Sample initial pH value is 6.00~7.00.When experiment, 50mg adsorbent, room temperature, revolving speed 100~150 are added in every 100mL waste water
Under the conditions of rev/min, after vibrating 2h, Magneto separate takes 2~3mL supernatant, using residual in ultraviolet specrophotometer measurement solution
The dyes concentration that stays simultaneously calculates adsorption capacity, and calculation formula is as follows:
In formula: the adsorption capacity of dyestuff, mg/g when qe is balance；V is wastewater volume, L；C0 is dyestuff initial concentration,
mg/L；Ce is the equilibrium concentration of dyestuff, mg/L；M is the quality of adsorbent, g.
Experimental result indicates, at 25 DEG C, adsorbent is 115.20mg/g, device to hole to methylene blue maximum adsorption capacity
Sparrow malachite green maximum adsorption capacity is 151.50mg/g.
Embodiment 2
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) 2.00g (0.005mol) Fe is weighed respectively2(SO4)3, 1.20g (0.02mol) SiO 2 powder and 1.55g
(0.0055mol)FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:SiO2=1.8:1:3.6.First by Fe2(SO4)3With two
Silicon oxide powder is added in 100ml deionized water, ultrasonic disperse 10min, then magnetic agitation, to being completely dissolved, whipping temp is
60 DEG C, FeSO is then added4·7H2O stirring a few minutes make ferrous ion be completely dissolved to obtain mixed solution.
(2) sodium hydroxide 1.6g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring adjusts pH to 11, and temperature is controlled at 60 DEG C, reacted 120 minutes by heating, stops heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying grinds porous up to magnetic silica in a vacuum drying oven after 12 hours
High-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 2
Ionic dye waste water measures its absorption property to dyestuff.Prepare the simulated wastewater that dye solution is 10-100mg/L, waste water
Sample initial pH value is 6.00~7.00.When experiment, 50mg adsorbent, room temperature, revolving speed 100~150 are added in every 100mL waste water
Under the conditions of rev/min, after vibrating 2h, Magneto separate takes 2~3mL supernatant, using residual in ultraviolet specrophotometer measurement solution
The dyes concentration that stays simultaneously calculates adsorption capacity, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
121.23mg/g is 163.52mg/g to malachite green maximum adsorption capacity.
Embodiment 3
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) Fe is weighed respectively2(SO4)3, SiO 2 powder and FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:
SiO2=2:1:3.First by Fe2(SO4)3It is added in 100ml deionized water with SiO 2 powder, ultrasonic disperse 10min, then magnetic
Power is stirred to being completely dissolved, and whipping temp is 70 DEG C, and FeSO is then added4·7 H2O stirring a few minutes keep ferrous ion complete
Dissolution obtains mixed solution.
(2) sodium hydroxide 1.6g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring, heating adjust pH to 11, and temperature is controlled at 70 DEG C, is reacted 120 minutes, stop heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying grinds porous up to magnetic silica in a vacuum drying oven after 12 hours
High-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 3
Ionic dye waste water measures its absorption property to dyestuff.Prepare the simulated wastewater that dye solution is 10-100mg/L, waste water
Sample initial pH value is 6.00~7.00.When experiment, 50mg adsorbent, room temperature, revolving speed 100~150 are added in every 100mL waste water
Under the conditions of rev/min, after vibrating 2h, Magneto separate takes 2~3mL supernatant, using residual in ultraviolet specrophotometer measurement solution
The dyes concentration that stays simultaneously calculates adsorption capacity, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
108.61mg/g is 141.30mg/g to malachite green maximum adsorption capacity.
Embodiment 4
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) Fe is weighed respectively2(SO4)3, SiO 2 powder and FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:
SiO2=2:1:6.First by Fe2(SO4)3It is added in 100ml deionized water with SiO 2 powder, ultrasonic disperse 10min, then magnetic
Power is stirred to being completely dissolved, and whipping temp is 80 DEG C, and FeSO is then added4·7 H2O stirring a few minutes keep ferrous ion complete
Dissolution obtains mixed solution.
(2) sodium hydroxide 1.6g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring, heating adjust pH to 12, and temperature is controlled at 80 DEG C, is reacted 120 minutes, stop heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying grinds porous up to magnetic silica in a vacuum drying oven after 12 hours
High-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 3
Ionic dye waste water measures its absorption property to dyestuff.Prepare the simulated wastewater that dye solution is 10-100mg/L, waste water
Sample initial pH value is 6.00~7.00.When experiment, 50mg adsorbent, room temperature, revolving speed 100~150 are added in every 100mL waste water
Under the conditions of rev/min, after vibrating 2h, Magneto separate takes 2~3mL supernatant, using residual in ultraviolet specrophotometer measurement solution
The dyes concentration that stays simultaneously calculates adsorption capacity, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
116.97mg/g is 155.06mg/g to malachite green maximum adsorption capacity.
Embodiment 5
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) Fe is weighed respectively2(SO4)3, SiO 2 powder and FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:
SiO2=2:1:2.First by Fe2(SO4)3It is added in 100ml deionized water with SiO 2 powder, ultrasonic disperse 10min, then magnetic
Power is stirred to being completely dissolved, and whipping temp is 60 DEG C, and FeSO is then added4·7 H2O stirring a few minutes keep ferrous ion complete
Dissolution obtains mixed solution.
(2) sodium hydroxide 1.6g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring, heating adjust pH to 10, and temperature is controlled at 60 DEG C, is reacted 120 minutes, stop heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying grinds porous up to magnetic silica in a vacuum drying oven after 12 hours
High-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 3
Ionic dye waste water measures its absorption property to dyestuff.Prepare the simulated wastewater that dye solution is 10-100mg/L, waste water
Sample initial pH value is 6.00~7.00.When experiment, 50mg adsorbent, room temperature, revolving speed 100~150 are added in every 100mL waste water
Under the conditions of rev/min, after vibrating 2h, Magneto separate takes 2~3mL supernatant, using residual in ultraviolet specrophotometer measurement solution
The dyes concentration that stays simultaneously calculates adsorption capacity, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
96.59mg/g is 114.85mg/g to malachite green maximum adsorption capacity.
Embodiment 6
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) Fe is weighed respectively2(SO4)3, SiO 2 powder and FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:
SiO2=1.8:1:4.5.First by Fe2(SO4)3It is added in 100ml deionized water with SiO 2 powder, ultrasonic disperse 10min,
For magnetic agitation to being completely dissolved, whipping temp is 60 DEG C again, and FeSO is then added4·7 H2O stirring a few minutes make ferrous ion
It is completely dissolved to obtain mixed solution.
(2) sodium hydroxide 1.6g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring, heating adjust pH to 11, and temperature is controlled at 60 DEG C, is reacted 120 minutes, stop heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying grinds porous up to magnetic silica in a vacuum drying oven after 12 hours
High-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 3
Ionic dye waste water measures its absorption property to dyestuff.Prepare the simulated wastewater that dye solution is 10-100mg/L, waste water
Sample initial pH value is 6.00~7.00.When experiment, 50mg adsorbent, room temperature, revolving speed 100~150 are added in every 100mL waste water
Under the conditions of rev/min, after vibrating 2h, Magneto separate takes 2~3mL supernatant, using residual in ultraviolet specrophotometer measurement solution
The dyes concentration that stays simultaneously calculates adsorption capacity, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
114.50mg/g is 138.54mg/g to malachite green maximum adsorption capacity.
Above-described embodiment illustrates that preparation process of the present invention is easy, environmental protection, at low cost, the porous height of gained magnetic silica
It is good to Adsorption dye of positive ion effect to imitate adsorbent, adsorption capacity is high, is a kind of efficient absorption for removing dyeing waste water
Agent has biggish use value in the market.
Comparative example 1
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) 2.00g (0.005mol) Fe is weighed respectively2(SO4)3, 1.20g (0.02mol) SiO 2 powder and 1.40g
(0.005mol)FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:SiO2=2:1:4.First by Fe2(SO4)3And silica
Powder is added in 100ml deionized water, ultrasonic disperse 10min, then magnetic agitation, to being completely dissolved, whipping temp is 60 DEG C, so
Afterwards plus FeSO4·7H2O stirring a few minutes make ferrous ion be completely dissolved to obtain mixed solution.
(2) sodium hydroxide 1.60g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring adjusts pH to 9, and temperature is controlled at 60 DEG C, reacted 120 minutes by heating, stops heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying is ground after 12 hours up to Fe in a vacuum drying oven3+:SiO2The magnetic of=1:2
Property porous silica high-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 1
Ionic dye waste water measures its absorption property to dyestuff, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
59.65mg/g is 62.54mg/g to malachite green maximum adsorption capacity.
Comparative example 2
A kind of preparation method of magnetic silica porous adsorbent, includes the following steps:
(1) 2.00g (0.005mol) Fe is weighed respectively2(SO4)3, 1.20g (0.02mol) SiO 2 powder and 1.40g
(0.005mol)FeSO4·7H2O, molar concentration rate Fe3+:Fe2+:SiO2=2:1:4.First by Fe2(SO4)3And silica
Powder is added in 100ml deionized water, ultrasonic disperse 10min, then magnetic agitation, to being completely dissolved, whipping temp is 60 DEG C, so
Afterwards plus FeSO4·7H2O stirring a few minutes make ferrous ion be completely dissolved to obtain mixed solution.
(2) sodium hydroxide 1.60g is weighed, is dissolved in 300ml deionized water, temperature is controlled at 60 DEG C, as reaction
Aqueous slkali.
(3) mixed solution in 1 step is slowly added to in the aqueous slkali in 2 steps, mixed solution has been added subsequent
Continuous stirring adjusts pH to 13, and temperature is controlled at 60 DEG C, reacted 120 minutes by heating, stops heating, and ageing is washed after 1 hour
Filtering to solution ph is neutrality, and air drying is ground after 12 hours up to Fe in a vacuum drying oven3+:SiO2The magnetic of=1:2
Property porous silica high-efficiency adsorbent.
The fellatio of the powder porous high-efficiency adsorbent treatment of laboratory simulation of magnetic silica made from Application Example 1
Ionic dye waste water measures its absorption property to dyestuff, and at 25 DEG C, adsorbent is to methylene blue maximum adsorption capacity
65.45mg/g is 72.82mg/g to malachite green maximum adsorption capacity.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (9)
1. a kind of preparation method of magnetic silica porous adsorbent, which comprises the steps of: by silica
Powder and ferric ion solutions mixing, are added 60~80 DEG C of hot alkaline solution, adjust pH to 10.00~12.00, sufficiently drop after reaction
To room temperature ageing, washing to neutrality, drying and grinding obtains magnetic silica porous adsorbent,
Wherein ferric iron and ferrous molar ratio are 1.8~2.0:1 in ferric ion solutions, SiO 2 powder with it is ferric
Molar ratio is 1~3:1, and reaction temperature is 60~80 DEG C, 60~120min of reaction time.
2. preparation method as described in claim 1, which is characterized in that the SiO 2 powder is 2 with ferric molar ratio
~3:1.
3. preparation method as claimed in claim 2, which is characterized in that the pH is adjusted to 11~12.
4. preparation method as claimed in claim 3, which is characterized in that the ferric iron and ferrous molar ratio are 1.8:1, two
Silicon oxide powder and ferric molar ratio are 2:1, and pH is adjusted to 11, and reaction temperature is 60 DEG C.
5. preparation method as claimed in claim 3, which is characterized in that the ferric iron and ferrous molar ratio are 2:1, dioxy
SiClx powder and ferric molar ratio are 3:1, and pH is adjusted to 12, and reaction temperature is 80 DEG C.
6. the preparation method as described in Claims 1 to 5 any one, which is characterized in that the digestion time is 1~3h.
7. the magnetic silica porous adsorbent that preparation method described in Claims 1 to 5 any one is prepared.
8. the answering in the Adsorption dyeing waste water dye of positive ion of magnetic silica porous adsorbent described in claim 7
With.
9. application as claimed in claim 8, which is characterized in that the dye of positive ion is methylene blue and malachite green.
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| CN101499348A (en) * | 2008-10-30 | 2009-08-05 | 同济大学 | Hollow silicon dioxide/magnetic composite microsphere and its production method |
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