CN106824053A - A kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff - Google Patents
A kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff Download PDFInfo
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- CN106824053A CN106824053A CN201710219660.2A CN201710219660A CN106824053A CN 106824053 A CN106824053 A CN 106824053A CN 201710219660 A CN201710219660 A CN 201710219660A CN 106824053 A CN106824053 A CN 106824053A
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- fly ash
- based adsorbent
- preparation
- efficient absorption
- adsorbent
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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
- B01J20/10—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
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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
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/10—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- 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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/425—Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to fields such as environment, trade waste treatment, industrial pollution emission reductions, specially a kind of efficient absorption dye of positive ion is (such as：Methylene blue, crystal violet etc.) fly ash-based adsorbent preparation method.The method is concretely comprised the following steps：With flyash, SiO2As raw material, ammoniacal liquor and template are added, fly ash-based adsorbent is synthesized using alkali fusion hydrothermal synthesis method, the adsorbent has excellent absorption property for dyestuffs such as methylene blue, crystal violets.The method is not only the high value added utilization of flyash, additionally provides a kind of effective mode for administering waste water from dyestuff, and with good economy.
Description
Technical field
The present invention relates to the fields such as environment, trade waste treatment, industrial pollution emission reduction, specially a kind of efficient absorption sun
Ionic dye is (such as：Methylene blue, crystal violet etc.) fly ash-based adsorbent preparation method.
Background technology
Waste water from dyestuff is the waste water that a class gives off during production dyestuff and pigment.Due to the discharge capacity of waste water from dyestuff
With intermittence, water quality is unstable, belongs to very intractable industrial wastewater for big and discharge.According to statistics, whole world production per annual meeting
More than 700000 tons of more than 10000 kinds of dyestuffs, wherein 20% dyestuff can in textile dyeing and last handling process without
Any treatment is just taken as industrial wastewater to discharge.The species of dyestuff is various, and wherein the dye of positive ion is a kind of easy in aqueous
It is dissociated into the dyestuff of positively charged coloured ion.The good water solubility of the dye of positive ion, molecular weight be small and binding ability of hydrone
By force, waste component complexity, salinity and the COD contents that it is produced are high, and in acidity, and colourity can reach tens of thousands of times to hundreds of thousands
Times, it is difficult to biochemical degradation.
In numerous methods for the treatment of waste water from dyestuff, physisorphtion is simple and easy to do, floor space is small, treatment effect is aobvious
Write.The core technology of physisorphtion is the preparation of adsorbent.For example, activated carbon is good Absorbent, and to sun
The adsorbance of ionic dye is considerable.But activated carbon manufacturing cost higher is limited to, it is larger that resistance is promoted in commercialization.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff, with fine coal
Ash is raw material, and the fly ash-based adsorbent synthesized using alkali fusion hydrothermal synthesis method is had to cations such as methylene blue, crystal violets
Very efficient absorption property, process is simple, low production cost with high added value, and is conducive to environmental protection.
The technical scheme is that：
A kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff, comprises the following steps：
(1) after flyash is mixed with silicon source, highly basic according to Si/Al mol ratio=1~25, sode ash mass ratio 0.5~2,
1~2h of high-temperature roasting at 450 DEG C~600 DEG C, obtains clinker；
(2) clinker is 1 according to clinker, ammoniacal liquor and template weight ratio after cooling down mill-drying and purifying:1~2:0.1~
0.3 add ammoniacal liquor and template, and stir 2~4h, using weak acid adjust mixed liquor pH value be 9~12, and continue stirring 2~
8h；
(3) mixed liquor is transferred in autoclave, 48~90h of crystallization at 90~130 DEG C, through filtering, washing, is done
It is put into high temperature furnace after dry, is heated to 350 DEG C~600 DEG C 3~10h of roasting, goes template agent removing to obtain fly ash-based adsorbent.
The preparation method of the fly ash-based adsorbent of described efficient absorption dyestuff, the highly basic described in step (1) is hydrogen-oxygen
Change potassium or NaOH.
The preparation method of the fly ash-based adsorbent of described efficient absorption dyestuff, the silicon source described in step (1) is dioxy
SiClx or sodium metasilicate.
The preparation method of the fly ash-based adsorbent of described efficient absorption dyestuff, the template described in step (2) is ten
Six alkyl trimethyl ammonium bromide CTAB, described weak acid is glacial acetic acid.
The preparation method of the fly ash-based adsorbent of described efficient absorption dyestuff, fly ash-based adsorbent has very high
Methylene blue adsorption capacity, in pH value in the range of 2~11, temperature exists in the range of 30~60 DEG C to methylene blue clearance
More than 70%, the methylene blue adsorption capacity of sample is in more than 1000mg/g.
The preparation method of the fly ash-based adsorbent of described efficient absorption dyestuff, fly ash-based adsorbent is contaminated crystal violet
Material have adsorption capacity higher, in pH value in the range of 2~11, temperature in the range of 30~60 DEG C, to crystal violet clearance
More than 70%, the crystal violet adsorption capacity of sample is in more than 350mg/g.
Advantages of the present invention and beneficial effect are：
1st, the present invention is using flyash as raw material, and the adsorbent prepared using alkali fusion hydrothermal synthesis method is not only efficient
Commercial cationic adsorption capacity, and there is the incomparable huge advantage of other adsorbents in economy and the feature of environmental protection, can
It is widely used in the improvement of dye of positive ion sewage.
2nd, the inventive method gained fly ash-based adsorbent has methylene blue adsorption capacity very high, and methylene blue is gone
Except rate can even reach more than 90%, the methylene blue adsorption capacity of sample even can exceed 1300mg/g.In addition, flyash
Base adsorbent has adsorption capacity higher to Crystal Violet Dye.
Specific embodiment
In specific implementation process, the ultraviolet-visible spectrophotometric produced using Shanghai Precision Scientific Apparatus Co., Ltd
Meter (model 723N) determines concentration of the adsorbent to dyestuff in supernatant before and after Dye Adsorption, and calculates adsorption rate and equilibrium adsorption
Amount.
Below, the present invention is further elaborated on by embodiment.
Embodiment 1
In the present embodiment, the silica alumina ratio of mixture is adjusted to 5 by flyash addition silica:1, then with sode ash
Mass ratio 1:1.25 ratio addition NaOH, 1h is melted after mixing at 500 DEG C, obtains light green solid；Room temperature is cooled to, is ground
Wear into fine powder；After the fine powder and water that will be obtained are mixed with the ratio that liquid-solid ratio is 8,12h is stirred at room temperature, obtains clinker.Press
Weight ratio according to clinker, ammoniacal liquor and template CTAB is 1:1.4:0.2 adds ammoniacal liquor and template, and stirs 3h, uses ice second
Acid adjustment mixed liquor pH value is 10.5, and continues to stir 3h；Mixture is transferred in autoclave, the crystallization at 120 DEG C
60h, is put into high temperature furnace after filtering, washing, dry and is first heated to 350 DEG C of roasting 3h, goes template agent removing to obtain fly ash base
Adsorbent.
Test finds that gained fly ash-based adsorbent reaches 71% to the adsorption rate of methylene blue solution and crystal violet solution
With 82%, 1075mg/g and 386mg/g are respectively to the equilibrium adsorption capacity of the two.
Embodiment 2
In the present embodiment, the silica alumina ratio of mixture is adjusted to 10 by flyash addition silica:1, then with alkali
Grey mass ratio 1:1.5 ratio addition NaOH, 1h is melted after mixing at 550 DEG C, obtains light green solid；It is cooled to room temperature,
Grind to form fine powder；After the fine powder and water that will be obtained are mixed with the ratio that liquid-solid ratio is 8,24h is stirred at room temperature, obtains clinker.
Weight ratio according to clinker, ammoniacal liquor and template CTAB is 1:1.4:0.2 adds ammoniacal liquor and template, and stirs 3h, uses ice
Acetic acid adjustment mixed liquor pH value is 12, and continues to stir 3h；Mixture is transferred in autoclave, the crystallization at 110 DEG C
72h, is put into high temperature furnace after filtering, washing, dry and is first heated to 450 DEG C of roasting 4h, goes template agent removing to obtain fly ash base
Adsorbent.
Test finds that gained fly ash-based adsorbent reaches 80% to the adsorption rate of methylene blue solution and crystal violet solution,
1850mg/g and 435mg/g are respectively to the equilibrium adsorption capacity of the two.
Embodiment result shows that the present invention is with flyash, SiO2As raw material, ammoniacal liquor and template are added, using alkali fusion
Hydrothermal synthesis method synthesizes fly ash-based adsorbent, and the adsorbent has excellent absorption property for dyestuffs such as methylene blues.Should
Method is not only the high value added utilization of flyash, additionally provides a kind of mode of effective improvement waste water from dyestuff, and have
Good economy.
Claims (6)
1. a kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff, it is characterised in that comprise the following steps：
(1) after flyash is mixed with silicon source, highly basic according to Si/Al mol ratio=1~25, sode ash mass ratio 0.5~2,450
DEG C~600 DEG C at 1~2h of high-temperature roasting, obtain clinker；
(2) clinker is 1 according to clinker, ammoniacal liquor and template weight ratio after cooling down mill-drying and purifying:1~2:0.1~0.3
Ammoniacal liquor and template are added, and stirs 2~4h, it is 9~12 to adjust mixed liquor pH value using weak acid, and continues 2~8h of stirring；
(3) mixed liquor is transferred in autoclave, 48~90h of crystallization at 90~130 DEG C, after filtering, washing, drying
It is put into high temperature furnace, is heated to 350 DEG C~600 DEG C 3~10h of roasting, goes template agent removing to obtain fly ash-based adsorbent.
2. the preparation method of the fly ash-based adsorbent of efficient absorption dyestuff according to claim 1, it is characterised in that step
Suddenly the highly basic described in (1) is potassium hydroxide or NaOH.
3. the preparation method of the fly ash-based adsorbent of efficient absorption dyestuff according to claim 1, it is characterised in that step
Suddenly the silicon source described in (1) is silica or sodium metasilicate.
4. the preparation method of the fly ash-based adsorbent of efficient absorption dyestuff according to claim 1, it is characterised in that step
Suddenly the template described in (2) is cetyl trimethylammonium bromide CTAB, and described weak acid is glacial acetic acid.
5. the preparation method of the fly ash-based adsorbent of efficient absorption dyestuff according to claim 1, it is characterised in that powder
Coal ash base adsorbent has methylene blue adsorption capacity very high, and in pH value in the range of 2~11, temperature is in 30~60 DEG C of scopes
Interior, to methylene blue clearance more than 70%, the methylene blue adsorption capacity of sample is in more than 1000mg/g.
6. the preparation method of the fly ash-based adsorbent of efficient absorption dyestuff according to claim 1, it is characterised in that powder
Coal ash base adsorbent has adsorption capacity higher to Crystal Violet Dye, and in pH value in the range of 2~11, temperature is at 30~60 DEG C
In the range of, to crystal violet clearance more than 70%, the crystal violet adsorption capacity of sample is in more than 350mg/g.
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| CN201710219660.2A CN106824053A (en) | 2017-04-06 | 2017-04-06 | A kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff |
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| CN201710219660.2A CN106824053A (en) | 2017-04-06 | 2017-04-06 | A kind of preparation method of the fly ash-based adsorbent of efficient absorption dyestuff |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430029A (en) * | 2021-06-23 | 2021-09-24 | 太原理工大学 | Method for hydrophobic modification of surface of low-rank coal by mechanochemical method |
| CN116603504A (en) * | 2023-05-29 | 2023-08-18 | 中国矿业大学 | Method for synthesizing porous carbon-silicon composite material from coal gasification fine slag and application thereof |
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2017
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430029A (en) * | 2021-06-23 | 2021-09-24 | 太原理工大学 | Method for hydrophobic modification of surface of low-rank coal by mechanochemical method |
| CN116603504A (en) * | 2023-05-29 | 2023-08-18 | 中国矿业大学 | Method for synthesizing porous carbon-silicon composite material from coal gasification fine slag and application thereof |
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Application publication date: 20170613 |