CN104289183A - Preparation method of nickel-aluminum hydrotalcite capable of adsorbing Congo red in dye wastewater - Google Patents
Preparation method of nickel-aluminum hydrotalcite capable of adsorbing Congo red in dye wastewater Download PDFInfo
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- CN104289183A CN104289183A CN201410529764.XA CN201410529764A CN104289183A CN 104289183 A CN104289183 A CN 104289183A CN 201410529764 A CN201410529764 A CN 201410529764A CN 104289183 A CN104289183 A CN 104289183A
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- nickel
- aluminum hydrotalcite
- congo red
- dye wastewater
- waste water
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- 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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- 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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of nickel-aluminum hydrotalcite capable of adsorbing Congo red in dye wastewater. The preparation method of the nickel-aluminum hydrotalcite capable of adsorbing Congo red in the dye wastewater comprises the following steps: firstly weighing 0.009mol of nickel phosphate and 0.003mol of aluminium nitrate, diluting the nickel phosphate and the aluminium nitrate in 80mL of absolute ethyl alcohol solution containing 0.04mol of carbamide, stirring at the room temperature for one hour, performing hydrothermal reaction, then reacting at 100 DEG C for 12 hours, cooling the solution to the room temperature, removing ions by ethyl alcohol and washing, and drying at 60 DEG C for 6 hours; calcining the solution at 500 DEG C for 2 hours in a boiling furnace, then adding sodium dodecyl benzene sulfonate and soaking in acetic acid alcohol solution for 12 hours; and then putting the solution in a constant-temperature furnace, and drying at 105 DEG C, and thus obtaining the nickel-aluminum hydrotalcite. An application of the nickel-aluminum hydrotalcite comprises the following steps: taking 10L of dye wastewater, detecting the dye wastewater to obtain a chromaticity of 15 and a pH value of 10, adding the dye wastewater in a vessel, then wrapping the nickel-aluminum hydrotalcite with gauze, putting the nickel-aluminum hydrotalcite in the vessel, stirring for 2 minutes, then precipitating for 3 minutes. Through detection, chromaticity of the wastewater after adsorption is 5, the pH value is 7 and the adsorption rate for Congo red in dye wastewater is greater than 95%.
Description
Technical field
The present invention relates to Congo red nickel aluminum hydrotalcite preparation method in a kind of absorbing dye waste water, belong to field of environment protection.
Background technology
The development of textile industry has driven the development of DYE PRODUCTION, investigation shows that dyestuff that the whole world produces every year is more than 700,000 tons, wherein 2% directly enters water body discharges with the form of waste water, waste water from dyestuff complicated component, change of water quality is large, colourity is dark, concentration is large, difficult treatment, especially in waste water from dyestuff containing a large amount of Congo red.
Congo red, chemistry is by name: diphenyl-4,4 '-two (azo-2-)-1-amino naphthalenes-4-sodium sulfonate, and molecular formula is C32H22N6Na2O6S2, is brown-red powder, and water-soluble in yellowish red color, it is orange for being dissolved in alcohol.For as acid-base indicator, color change interval is 3.5 to 5.2, and alkali state is red, and acid-state is bluish violet.For diagnosis starch pathology, inject in latter 1 hour and be no more than 40% from blood plasma discharge, it is normal for draining also aobvious author in urine, and as discharged more than 60% in blood plasma, discharging still aobvious author in urine then may have amyloid pathology.As Congo red in a large number in having in urine, the renal tubule fatty pathology that expressed possibility or similar pathology.What contain in waste water from dyestuff Congo redly also exists carcinogenic, to damage non-natus danger, therefore explores a kind of effective and economic being significant to environmental protection for processing method Congo red in absorbing dye waste water.
At present, have a lot to the processing method of dyeing waste water both at home and abroad, mainly contain absorption method, flocculence, Ozonation etc., wherein absorption method utilizes the suction-operated of pollutant in Adsorbent For Removal of Heavy to remove pollutant, adsorbent is porous material, having very large specific area, is generally utilize active carbon to adsorb for adsorbent.Flocculence is in waste water, add certain material, by the effect of physics or chemistry, make former water-soluble or in trickle state the pollutant of not free settling, filtration, be combined into larger particles, so that the method be separated.Ozonation be oxidant based on ozone, ozone is better to the decolorizing effect of most dyestuff, non-secondary pollution.
At present, the synthetic method of hydrotalcite also only rests on traditional coprecipitation stage.
Summary of the invention
The object of the present invention is to provide Congo red nickel aluminum hydrotalcite preparation method in a kind of absorbing dye waste water, realize recycling economy, cleaner production, the effects such as the low and percent of decolourization of expense is high.
Congo red nickel aluminum hydrotalcite preparation method in a kind of absorbing dye waste water provided by the invention to achieve these goals, its method is:
(1) first take 0.009mol nickel phosphate, 0.003mol aluminum nitrate is diluted in 80mL and contains in the ethanol solution of 0.04mol urea, stir 1h at ambient temperature;
(2) at condition is 100 DEG C ~ 150 DEG C, 12 ~ 14h is reacted after pouring hydro-thermal reaction into, under temperature reaches room temperature after cooling;
(3) remove deionization with ethanol and clean for several times with water, dry 6 ~ 8h at 60 DEG C;
(4) sample obtained is calcined 2 ~ 4h boiling in stove at 500 DEG C ~ 600 DEG C, opening warm speed is 2 DEG C/min;
(5) drop into neopelex after calcining and soak 12 ~ 24h in vinyl alcohol solution;
(6) dry at temperature is 105 DEG C in constant temperature oven after soaking and can obtain nickel aluminum hydrotalcite.
Neopelex in described vinyl alcohol solution is 0.1 ~ 0.5mol/L.
In a kind of absorbing dye waste water, the application process of Congo red nickel aluminum hydrotalcite is:
First get 10 ~ 20L waste water from dyestuff to detect, to record its colourity be 15 ~ 20, pH is 10 ~ 15, is put into by waste water from dyestuff in vessel, then the vessel that waste water from dyestuff is housed are put into after nickel aluminum hydrotalcite gauze being wrapped up three layers, carry out stirring 2 ~ 4min, then precipitate 3 ~ 5min, the gauze of visible parcel nickel aluminum hydrotalcite becomes yellowish red color from white, again the waste water after hydrotalcite absorption is detected, to record its colourity be 5 ~ 6, pH is 7 ~ 7.5, and adsorption rate is more than 95%.
Significant advantage of the present invention is:
(1) neopelex adopted can change its surface texture, increases absorption property and surface polarity, has certain suction-operated, thus reach the effect of purification in waste water to organic matter.
(2) hydrotalcite has good absorption property, can while synthetic hydrotalcite the waste water from dyestuff of adsorption cleaning congolite.
Detailed description of the invention
Congo red nickel aluminum hydrotalcite preparation method in a kind of absorbing dye waste water, its method is:
First take 0.009mol nickel phosphate, 0.003mol aluminum nitrate is diluted in 80mL and contains in the ethanol solution of 0.04mol urea, stir 1h at ambient temperature; At condition is 100 DEG C ~ 150 DEG C, 12 ~ 14h is reacted, under temperature reaches room temperature after cooling after pouring hydro-thermal reaction into; Remove deionization with ethanol and clean for several times with water, dry 6 ~ 8h at 60 DEG C; The sample obtained is calcined 2 ~ 4h boiling in stove at 500 DEG C ~ 600 DEG C, and opening warm speed is 2 DEG C/min; Drop into neopelex after calcining and soak 12 ~ 24h in vinyl alcohol solution; Dry at temperature is 105 DEG C in constant temperature oven after immersion and can obtain nickel aluminum hydrotalcite.
Neopelex in described vinyl alcohol solution is 0.1 ~ 0.5mol/L.
Below by example, the present invention is elaborated:
Example 1
First take 0.009mol nickel phosphate, 0.003mol aluminum nitrate is diluted in 80mL and contains in the ethanol solution of 0.04mol urea, stir 1h at ambient temperature; At condition is 100 DEG C, 12h is reacted, under temperature reaches room temperature after cooling after pouring hydro-thermal reaction into; Remove deionization with ethanol and clean for several times with water, dry 6h at 60 DEG C; The sample obtained is calcined 2h boiling in stove at 500 DEG C, and opening warm speed is 2 DEG C/min; Dropping into neopelex after calcining is that 0.1mol/L soaks 12h in vinyl alcohol solution; Dry at temperature is 105 DEG C in constant temperature oven after immersion and can obtain nickel aluminum hydrotalcite.
Process the waste water that certain dyestuff factory is flowed out, first get 10L waste water from dyestuff and detect, recording its colourity is 15, pH is 10, is put into by waste water from dyestuff in vessel, puts into the vessel that waste water from dyestuff is housed after then nickel aluminum hydrotalcite gauze being wrapped up three layers, carry out stirring 2min, precipitate 3min again, the gauze of visible parcel nickel aluminum hydrotalcite becomes yellowish red color from white, then detects the waste water after hydrotalcite absorption, recording its colourity is 5, pH is 7, and adsorption rate is 95%, and reaching can discharge standard.
Example 2
First take 0.009mol nickel phosphate, 0.003mol aluminum nitrate is diluted in 80mL and contains in the ethanol solution of 0.04mol urea, stir 1h at ambient temperature; At condition is 120 DEG C, 13h is reacted, under temperature reaches room temperature after cooling after pouring hydro-thermal reaction into; Remove deionization with ethanol and clean for several times with water, dry 7h at 60 DEG C; The sample obtained is calcined 3h boiling in stove at 550 DEG C, and opening warm speed is 2 DEG C/min; Dropping into neopelex after calcining is that 0.3mol/L soaks 18h in vinyl alcohol solution; Dry at temperature is 105 DEG C in constant temperature oven after immersion and can obtain nickel aluminum hydrotalcite.
The waste water that certain dyestuff factory is flowed out is processed, first get 15L waste water from dyestuff to detect, recording its colourity is 17, pH is 12, waste water from dyestuff is put in vessel, then the vessel that waste water from dyestuff is housed are put into after nickel aluminum hydrotalcite gauze being wrapped up three layers, carry out stirring 3min, precipitate 4min again, the gauze of visible parcel nickel aluminum hydrotalcite becomes yellowish red color from white, then detects the waste water after hydrotalcite absorption, recording its colourity is 5.5, pH is 7.2, and adsorption rate is 98%, and reaching can discharge standard.
Example 3
First take 0.009mol nickel phosphate, 0.003mol aluminum nitrate is diluted in 80mL and contains in the ethanol solution of 0.04mol urea, stir 1h at ambient temperature; At condition is 150 DEG C, 14h is reacted, under temperature reaches room temperature after cooling after pouring hydro-thermal reaction into; Remove deionization with ethanol and clean for several times with water, dry 8h at 60 DEG C; The sample obtained is calcined 4h boiling in stove at 600 DEG C, and opening warm speed is 2 DEG C/min; Dropping into neopelex after calcining is that 0.5mol/L soaks 24h in vinyl alcohol solution; Dry at temperature is 105 DEG C in constant temperature oven after immersion and can obtain nickel aluminum hydrotalcite.
The waste water that certain dyestuff factory is flowed out is processed, first get 20L waste water from dyestuff to detect, recording its colourity is 20, pH is 15, waste water from dyestuff is put in vessel, then the vessel that waste water from dyestuff is housed are put into after nickel aluminum hydrotalcite gauze being wrapped up three layers, carry out stirring 4min, precipitate 5min again, the gauze of visible parcel nickel aluminum hydrotalcite becomes yellowish red color from white, then detects the waste water after hydrotalcite absorption, recording its colourity is 6, pH is 7.5, and adsorption rate is more than 98%, and reaching can discharge standard.
Claims (2)
1. a Congo red nickel aluminum hydrotalcite preparation method in absorbing dye waste water, is characterized in that:
(1) first take 0.009mol nickel phosphate, 0.003mol aluminum nitrate is diluted in 80mL and contains in the ethanol solution of 0.04mol urea, stir 1h at ambient temperature;
(2) at condition is 100 DEG C ~ 150 DEG C, 12 ~ 14h is reacted after pouring hydro-thermal reaction into, under temperature reaches room temperature after cooling;
(3) remove deionization with ethanol and clean for several times with water, dry 6 ~ 8h at 60 DEG C;
(4) sample obtained is calcined 2 ~ 4h boiling in stove at 500 DEG C ~ 600 DEG C, opening warm speed is 2 DEG C/min;
(5) drop into neopelex after calcining and soak 12 ~ 24h in vinyl alcohol solution;
(6) dry at temperature is 105 DEG C in constant temperature oven after soaking and can obtain nickel aluminum hydrotalcite.
2. Congo red nickel aluminum hydrotalcite preparation method in a kind of absorbing dye waste water according to claim 1, is characterized in that: the neopelex in described vinyl alcohol solution is 0.1 ~ 0.5mol/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410529764.XA CN104289183A (en) | 2014-10-09 | 2014-10-09 | Preparation method of nickel-aluminum hydrotalcite capable of adsorbing Congo red in dye wastewater |
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| CN201410529764.XA CN104289183A (en) | 2014-10-09 | 2014-10-09 | Preparation method of nickel-aluminum hydrotalcite capable of adsorbing Congo red in dye wastewater |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787808A (en) * | 2015-04-16 | 2015-07-22 | 电子科技大学 | Synthetic method of nickel aluminum layered double hydroxide nano material |
| CN106044870A (en) * | 2016-08-22 | 2016-10-26 | 电子科技大学 | Lamellar nickel-aluminum hydrotalcite nanometer material preparation method |
| CN112657470A (en) * | 2020-12-03 | 2021-04-16 | 乌日娜 | Method for modifying hydrotalcite by using long carbon chain anionic surfactant |
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| CN1962046A (en) * | 2006-10-20 | 2007-05-16 | 山东大学 | A heavy metal ion absorbent and application thereof in removal of heavy metal ion |
| CN101829539A (en) * | 2010-05-21 | 2010-09-15 | 大连理工大学 | Method for preparing NiAl composite oxide desulfurizing agent with flower-shaped appearance |
| CN103285804A (en) * | 2013-05-16 | 2013-09-11 | 马玉山 | Preparation method of defluorinating adsorbent |
| CN103464090A (en) * | 2013-08-21 | 2013-12-25 | 青岛科技大学 | Red mud modification method, modified substance and application of modified substance in adsorption of brilliant blue dye |
-
2014
- 2014-10-09 CN CN201410529764.XA patent/CN104289183A/en active Pending
Patent Citations (4)
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| CN1962046A (en) * | 2006-10-20 | 2007-05-16 | 山东大学 | A heavy metal ion absorbent and application thereof in removal of heavy metal ion |
| CN101829539A (en) * | 2010-05-21 | 2010-09-15 | 大连理工大学 | Method for preparing NiAl composite oxide desulfurizing agent with flower-shaped appearance |
| CN103285804A (en) * | 2013-05-16 | 2013-09-11 | 马玉山 | Preparation method of defluorinating adsorbent |
| CN103464090A (en) * | 2013-08-21 | 2013-12-25 | 青岛科技大学 | Red mud modification method, modified substance and application of modified substance in adsorption of brilliant blue dye |
Non-Patent Citations (1)
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| 石雯 等: "十二烷基苯磺酸钠改性的镁铝水滑石吸附2，4-D除草剂的性能研究", 《科学技术与工程》, vol. 13, no. 1, 31 January 2013 (2013-01-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787808A (en) * | 2015-04-16 | 2015-07-22 | 电子科技大学 | Synthetic method of nickel aluminum layered double hydroxide nano material |
| CN106044870A (en) * | 2016-08-22 | 2016-10-26 | 电子科技大学 | Lamellar nickel-aluminum hydrotalcite nanometer material preparation method |
| CN112657470A (en) * | 2020-12-03 | 2021-04-16 | 乌日娜 | Method for modifying hydrotalcite by using long carbon chain anionic surfactant |
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Application publication date: 20150121 |