CN104289180A - Preparation and application of aerobic nitrification granular sludge activated carbon adsorbent - Google Patents
Preparation and application of aerobic nitrification granular sludge activated carbon adsorbent Download PDFInfo
- Publication number
- CN104289180A CN104289180A CN201410501452.8A CN201410501452A CN104289180A CN 104289180 A CN104289180 A CN 104289180A CN 201410501452 A CN201410501452 A CN 201410501452A CN 104289180 A CN104289180 A CN 104289180A
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- activated sludge
- granular activated
- aerobic nitrifying
- preparation
- nitrifying granular
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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
- B01J20/20—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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
- B01J20/28016—Particle form
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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
Abstract
The invention relates to preparation and application of an aerobic nitrification granular sludge activated carbon adsorbent. The preparation method provided by the invention comprises the following steps: drying, grinding and screening aerobic nitrification granular sludge, then activating by using a zinc chloride solution for 20-24h, placing into a quartz tube of a tubular furnace, firstly introducing nitrogen into the tubular furnace at room temperature for 1-2h, then heating the tubular furnace to 600-700 DEG C at the rate of 10-18 DEG C/min under the protection of the nitrogen, keeping for 0.5-1.5h, reducing the temperature to room temperature, then stopping the introduction of the nitrogen, taking out, washing off impurities with hydrochloric acid, repeatedly washing with deionized water till neutral, drying, grinding and screening to obtain aerobic nitrification granular sludge activated carbon. According to the invention, the method of using the activated carbon prepared from the aerobic nitrification granular sludge as the adsorbent is adopted for the first time and is simple and easy to operate, the adsorbent is low in cost, high in adsorption capacity and reusable, and can effectively treat a cationic dye solution, and secondary pollution can be avoided in an adsorption process.
Description
Technical field
The present invention relates to a kind of preparations and applicatio of aerobic nitrifying granular activated sludge acticarbon, be applicable to the removal of the dyeing waste water dye of positive ion, belong to technical field of active carbon.
Background technology
In recent years, the development of dye industry, while bringing colourful visual enjoyment for the mankind, also causes serious threat to the mankind and ecological environment.The dye of positive ion is take petrochemicals as primary raw material mostly, and through the aromatic compounds of Prof. Du Yucang, its stable chemical nature, biodegradability is low, has potential toxicity and carcinogenic, aberration inducing effect.Therefore, in ambient water the removal of dye discoloration more and more by people are paid close attention to.
Active carbon is a kind of common adsorbent, has abundant internal pore structure and high-specific surface area, has very strong adsorption selection ability, its successful, simple to operate.Therefore utilize the dye of positive ion in absorption method removal sewage, from efficiency and environmental protection aspect, all there is good application prospect.Aerobic nitrifying granular activated sludge is the graininess microorganism condensate with regular texture formed by the self-cohesion action of microorganism, is a kind of new and effective biological denitrificaion granule sludge technology grown up on the basis of anaerobic grain sludge.The dirty water living creature processing technique utilizing aerobic nitrifying granular activated sludge to carry out a new generation is the hot issue of Chinese scholars research always.Aerobic nitrifying granular activated sludge contains large amount of organic and the available resources such as protein-based, can change into carbon-bearing adsorbent.The active carbon that the present invention adopts aerobic nitrifying granular activated sludge to prepare first is simple as the method for adsorbent, with low cost, and adsorption capacity is high, can reuse, and can effectively process dye of positive ion solution, adsorption process does not cause secondary pollution.
Summary of the invention
The object of this invention is to provide a kind of aerobic nitrifying granular activated sludge acticarbon.The present invention also aims to provide a kind of active carbon to remove the method for water cationic dyestuff.
technical scheme of the present invention is as follows:
1. a preparation for aerobic nitrifying granular activated sludge acticarbon, step is as follows:
(1) by dry at 100 ~ 110 DEG C for the aerobic nitrifying granular activated sludge cultivated in the sbr reactor device of laboratory, grinding, 80 ~ 150 orders sieve, and obtain dewatered sludge powder;
(2) by dewatered sludge powder 2 ~ 6 mol/L zinc chloride activation 20 ~ 24 h; then tube furnace is put into; protection gas is made with nitrogen; at 600 ~ 700 DEG C, carbonize 0.5 ~ 1.5 h, the rate of heat addition controls, at 10 ~ 18 DEG C/min, to be cooled to room temperature; impurity is washed away with 2 ~ 4 mol/L hydrochloric acid; spend deionized water to neutral, dry to constant weight for 100 ~ 110 DEG C, obtained aerobic nitrifying granular activated sludge active carbon.
2. the cultivation of above-mentioned aerobic nitrifying granular activated sludge, artificial wastewater used provides carbon source with glucose, and ammonium chloride provides nitrogenous source, and sodium acid carbonate regulates pH 7.5 ~ 8.0, and influent COD is 500 ~ 800 mg/L, NH
4-N is 100 ~ 400 mg/L, and mud particle diameter is 1 ~ 3 mm.
3. aerobic nitrifying granular activated sludge acticarbon is used for a removal for water cationic dyestuff, and step is as follows:
(1) get 30 ~ 50 mL, 40 ~ 60 mg/L dye of positive ion solution in the conical flask of 250mL, add the aerobic nitrifying granular activated sludge active carbon of 6 ~ 16 mg, 20 ~ 40 DEG C are placed down in shaking table 1 ~ 2 h that vibrates, take out mixed liquor, centrifugal, get supernatant spectrophotometer measurement absorbance;
(2) draw the working curve of the concentration ~ absorbance of the dye of positive ion, find the concentration of the rear anions in solution dyestuff of absorption according to working curve
c e, according to the initial concentration of anions in solution dyestuff
c 0with the concentration of anions in solution dyestuff after absorption
c ecalculate dye of positive ion clearance.
The above-mentioned dye of positive ion is selected from one of following: methylene blue, malachite green, dimethyl diaminophenazine chloride, acridine orange.
useful achievement of the present invention
1. in the present invention, aerobic nitrifying granular activated sludge is a kind of novel material preparing active carbon;
2. the present invention can realize the efficient removal to the dye of positive ion under less active carbon dosage, and clearance reaches more than 95%;
3. the preparation technology of active carbon of the present invention is simple, small investment, and energy consumption is low;
4. the present invention adopt aerobic nitrifying granular activated sludge to prepare first active carbon as adsorbent, remarkably productive.
embodiment 1a kind of preparation method of aerobic nitrifying granular activated sludge acticarbon
(1) get the aerobic nitrifying granular activated sludge cultivated in the sbr reactor device of laboratory, cultivating artificial wastewater's influent COD used is 500 mg/L, NH
4-N is 100 mg/L, pH is 7.8, and particle diameter is 1 mm, dry at 103 DEG C, grinding, and 80 mesh sieve are sieved, and obtain dewatered sludge powder;
(2) by dewatered sludge powder 2 mol/L zinc chloride activation 20 h; then tube furnace is put into; protection gas is made with nitrogen; at 600 DEG C, carbonize 0.5 h, the rate of heat addition controls, at 10 DEG C/min, to be cooled to room temperature; impurity is washed away with 2 mol/L hydrochloric acid; spend deionized water to neutral, dry to constant weight for 103 DEG C, obtained aerobic nitrifying granular activated sludge active carbon.
embodiment 2a kind of preparation method of aerobic nitrifying granular activated sludge acticarbon
(1) get the aerobic nitrifying granular activated sludge cultivated in the sbr reactor device of laboratory, cultivating artificial wastewater's influent COD used is 650 mg/L, NH
4-N is 200 mg/L, pH is 7.8, and particle diameter is 2 mm, dry at 105 DEG C, grinding, and 100 mesh sieve are sieved, and obtain dewatered sludge powder;
(2) by dewatered sludge powder 5 mol/L zinc chloride activation 22 h; then tube furnace is put into; protection gas is made with nitrogen; at 650 DEG C, carbonize 1 h, the rate of heat addition controls, at 15 DEG C/min, to be cooled to room temperature; impurity is washed away with 3 mol/L hydrochloric acid; spend deionized water to neutral, dry to constant weight for 105 DEG C, obtained aerobic nitrifying granular activated sludge active carbon.
embodiment 3a kind of preparation method of aerobic nitrifying granular activated sludge acticarbon
(1) get the aerobic nitrifying granular activated sludge cultivated in the sbr reactor device of laboratory, cultivating artificial wastewater's influent COD used is 750 mg/L, NH
4-N is 300 mg/L, pH is 7.8, and particle diameter is 3mm, dry at 108 DEG C, grinding, and 150 mesh sieve are sieved, and obtain dewatered sludge powder;
(2) by dewatered sludge powder 6 mol/L zinc chloride activation 24 h; then tube furnace is put into; protection gas is made with nitrogen; at 700 DEG C, carbonize 1.5 h, the rate of heat addition controls, at 18 DEG C/min, to be cooled to room temperature; impurity is washed away with 4 mol/L hydrochloric acid; spend deionized water to neutral, dry to constant weight for 108 DEG C, obtained aerobic nitrifying granular activated sludge active carbon.
embodiment 4the removal of dye of positive ion methylene blue
(1) get 30 mL, 40 mg/L methylene blue solution in the conical flask of 250 mL, add the aerobic nitrifying granular activated sludge active carbon of 8 mg, 20 DEG C are placed down in shaking table 1 h that vibrates, and take out mixed liquor, centrifugal, get supernatant spectrophotometer measurement absorbance;
(2) draw the working curve of the concentration ~ absorbance of methylene blue, find the concentration of the rear Methylene Blue in Solution of absorption according to working curve
c e, according to the initial concentration of Methylene Blue in Solution
c 0with the concentration of Methylene Blue in Solution after absorption
c ecalculate methylene blue clearance, its clearance reaches 95.4%.
embodiment 5the removal of dye of positive ion malachite green
(1) get 35 mL, 45 mg/L malachite green solution in the conical flask of 250 mL, add the aerobic nitrifying granular activated sludge active carbon of 10 mg, 25 DEG C are placed down in shaking table 1.5 h that vibrate, and take out mixed liquor, centrifugal, get supernatant spectrophotometer measurement absorbance;
(2) draw the working curve of the concentration ~ absorbance of malachite green, find the concentration of the rear solution Malachite Green of absorption according to working curve
c e, according to the initial concentration of solution Malachite Green
c 0with the concentration of solution Malachite Green after absorption
c ecalculate malachite green clearance, its clearance reaches 96.5%.
embodiment 6the removal of dye of positive ion dimethyl diaminophenazine chloride
(1) get 45 mL, 55 mg/L neutral red solution in the conical flask of 250 mL, add the aerobic nitrifying granular activated sludge active carbon of 12 mg, 35 DEG C are placed down in shaking table 1.5 h that vibrate, and take out mixed liquor, centrifugal, get supernatant spectrophotometer measurement absorbance;
(2) draw the working curve of the concentration ~ absorbance of dimethyl diaminophenazine chloride, find the concentration of dimethyl diaminophenazine chloride in the rear solution of absorption according to working curve
c e, according to the initial concentration of dimethyl diaminophenazine chloride in solution
c 0with the concentration of dimethyl diaminophenazine chloride in solution after absorption
c ecalculate dimethyl diaminophenazine chloride clearance, its clearance reaches 96.0%.
embodiment 7the removal of dye of positive ion acridine orange
(1) get 50 mL, 60 mg/L acridine orange solution in the conical flask of 250 mL, add the aerobic nitrifying granular activated sludge active carbon of 14 mg, 40 DEG C are placed down in shaking table 2 h that vibrate, and take out mixed liquor, centrifugal, get supernatant spectrophotometer measurement absorbance;
(2) draw the working curve of the concentration ~ absorbance of acridine orange, find the concentration of acridine orange in the rear solution of absorption according to working curve
c e, according to the initial concentration of acridine orange in solution
c 0with the concentration of acridine orange in solution after absorption
c ecalculate acridine orange clearance, its clearance reaches 97.3%.
Claims (4)
1. a preparation for aerobic nitrifying granular activated sludge acticarbon, is characterized in that, comprises the following steps:
(1) by dry at 100 ~ 110 DEG C for the aerobic nitrifying granular activated sludge cultivated in the sbr reactor device of laboratory, grinding, 80 ~ 150 orders sieve, and obtain dewatered sludge powder;
(2) by dewatered sludge powder 2 ~ 6 mol/L zinc chloride activation 20 ~ 24 h; then tube furnace is put into; protection gas is made with nitrogen; at 600 ~ 700 DEG C, carbonize 0.5 ~ 1.5 h, the rate of heat addition controls, at 10 ~ 18 DEG C/min, to be cooled to room temperature; impurity is washed away with 2 ~ 4 mol/L hydrochloric acid; spend deionized water to neutral, dry to constant weight for 100 ~ 110 DEG C, obtained aerobic nitrifying granular activated sludge active carbon.
2. the preparation of a kind of aerobic nitrifying granular activated sludge acticarbon as claimed in claim 1, described aerobic nitrifying granular activated sludge, it is characterized in that, cultivate artificial wastewater used and provide carbon source with glucose, ammonium chloride provides nitrogenous source, sodium acid carbonate regulates pH 7.5 ~ 8.0, and influent COD is 500 ~ 800mg/L, NH
4-N is 100 ~ 400mg/L, and mud particle diameter is 1 ~ 3mm.
3. the preparation of a kind of aerobic nitrifying granular activated sludge acticarbon as claimed in claim 1, it is characterized in that, for the removal of water cationic dyestuff, step is as follows:
(1) get 30 ~ 50 mL, 40 ~ 60mg/L dye of positive ion solution in the conical flask of 250mL, add the aerobic nitrifying granular activated sludge active carbon of 6 ~ 16mg, 20 ~ 40 DEG C are placed down in shaking table 1 ~ 2 h that vibrates, take out mixed liquor, centrifugal, get supernatant spectrophotometer measurement absorbance;
(2) draw the working curve of the concentration ~ absorbance of the dye of positive ion, find the concentration of the rear anions in solution dyestuff of absorption according to working curve
c e, according to the initial concentration of anions in solution dyestuff
c 0with the concentration of anions in solution dyestuff after absorption
c ecalculate dye of positive ion clearance.
4. the preparation of a kind of aerobic nitrifying granular activated sludge acticarbon as claimed in claim 1, is characterized in that, the dye of positive ion is selected from one of following: methylene blue, malachite green, dimethyl diaminophenazine chloride, acridine orange.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104772143A (en) * | 2015-03-18 | 2015-07-15 | 昆明理工大学 | Preparation method of supported sludge-base catalyst for removing low-concentration carbon disulfide |
| CN106045002A (en) * | 2016-07-11 | 2016-10-26 | 华中科技大学 | Method for degrading organic substances or ammonia nitrogen by catalyzing persulfate through sludge biochar |
| CN110282624A (en) * | 2019-07-10 | 2019-09-27 | 广州市净水有限公司 | A method of active carbon is prepared using sludge |
| CN112827469A (en) * | 2021-01-08 | 2021-05-25 | 江西农业大学 | Preparation method of litsea cubeba nuclear-based magnetic activated carbon and application of litsea cubeba nuclear-based magnetic activated carbon in dye wastewater treatment |
| CN114524434A (en) * | 2022-04-09 | 2022-05-24 | 李立欣 | Method for preparing activated carbon by utilizing cavitated sludge |
Citations (3)
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| JP2008237997A (en) * | 2007-03-26 | 2008-10-09 | Sumitomo Heavy Ind Ltd | Waste water treatment apparatus |
| CN103013973A (en) * | 2012-12-17 | 2013-04-03 | 常州大学 | Method for preparing aerobiotic nitrifier immobilizing vector |
| CN103102007A (en) * | 2013-02-06 | 2013-05-15 | 东北林业大学 | Long-term storage method of aerobiotic nitrifying granule sludge |
-
2014
- 2014-09-27 CN CN201410501452.8A patent/CN104289180B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008237997A (en) * | 2007-03-26 | 2008-10-09 | Sumitomo Heavy Ind Ltd | Waste water treatment apparatus |
| CN103013973A (en) * | 2012-12-17 | 2013-04-03 | 常州大学 | Method for preparing aerobiotic nitrifier immobilizing vector |
| CN103102007A (en) * | 2013-02-06 | 2013-05-15 | 东北林业大学 | Long-term storage method of aerobiotic nitrifying granule sludge |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104772143A (en) * | 2015-03-18 | 2015-07-15 | 昆明理工大学 | Preparation method of supported sludge-base catalyst for removing low-concentration carbon disulfide |
| CN104772143B (en) * | 2015-03-18 | 2017-09-12 | 昆明理工大学 | For the preparation method for the support type sludge base catalyst for removing low concentration carbon disulfide |
| CN106045002A (en) * | 2016-07-11 | 2016-10-26 | 华中科技大学 | Method for degrading organic substances or ammonia nitrogen by catalyzing persulfate through sludge biochar |
| CN110282624A (en) * | 2019-07-10 | 2019-09-27 | 广州市净水有限公司 | A method of active carbon is prepared using sludge |
| CN112827469A (en) * | 2021-01-08 | 2021-05-25 | 江西农业大学 | Preparation method of litsea cubeba nuclear-based magnetic activated carbon and application of litsea cubeba nuclear-based magnetic activated carbon in dye wastewater treatment |
| CN114524434A (en) * | 2022-04-09 | 2022-05-24 | 李立欣 | Method for preparing activated carbon by utilizing cavitated sludge |
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