CN105776210A - Preparation method of distillers'grain-doped sludge activated carbon - Google Patents
Preparation method of distillers'grain-doped sludge activated carbon Download PDFInfo
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- CN105776210A CN105776210A CN201610306239.0A CN201610306239A CN105776210A CN 105776210 A CN105776210 A CN 105776210A CN 201610306239 A CN201610306239 A CN 201610306239A CN 105776210 A CN105776210 A CN 105776210A
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- distiller grains
- carbon
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- sludge
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- 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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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention relates to a preparation method of distillers'grain-doped sludge activated carbon and belongs to the field of sewage treatment. Aiming at a traditional sludge treatment method, the invention provides the preparation method of the distillers'grain-doped sludge activated carbon. The preparation method comprises the following steps of adopting sludge as a raw material; doping distillers'grain, and fermenting and concentrating by microwave under anaerobic conditions; pyrolyzing and carbonizing, and pretreating by a zinc chloride solution; then activating at high temperature, and washing and drying with a hydrochloric acid solution to obtain inexpensive activated carbon. According to the preparation method disclosed by the invention, zinc chloride has a dissolution effect for organic matters in the sludge at low temperature, so that original porosity is formed in the material; besides, the zinc chloride has certain catalytic dehydrating effect and supporting effect at high temperature, so that a framework is provided for newly-generated carbon when the sludge is carbonized; after inorganic components such as the zinc chloride and the like are dissolved and washed with the hydrochloric acid solution, the surface of carbon is exposed and becomes an active carbon porous structure with adsorption capacity; the preparation method is an effective method for enabling the sludge to realize resource stable utilization.
Description
Technical field
The preparation method that the present invention relates to a kind of distiller grains active sludge carbon that adulterates, belongs to sewage treatment area.
Background technology
Along with the reinforcement of the quickening of urbanization process, the increase of urban population and environmental consciousness, urban industry waste water is increasing with the discharge capacity of sanitary sewage, and treatment rate of domestic sewage also improves year by year, and the mud generation rate of Sewage Plant is also sharply increasing.The mud of sewage treatment plant is that moisture content is high, has the semi-drying solid waste with complicated rheological characteristic of substantial amounts of Organic substance, poisonous and harmful substance, its capacity corrupt, unstable, foul smelling big, easy, if do not dealt carefully with, will bring serious environmental pollution.Traditional mud mainly fills, burns, fills out sea and Land_use change, wherein fills, fills out sea and can not fundamentally solve the pollution problem of mud, burns cost high and can bring secondary pollution.Along with the increasingly stringent of environmental standard, the requirement to mud of Land_use change is also tightened up, it is necessary to the harm that the pollutant taking measures to alleviate in mud as far as possible bring, and the disposal of mud should be made to reach resource, stabilisation, innoxious target.
Summary of the invention
The technical problem to be solved: mainly fill for traditional mud, burn, fill out sea and Land_use change, wherein fill, fill out sea and can not fundamentally solve the pollution problem of mud, burn cost height and secondary pollution can be brought, soil is then easily polluted by Land_use change, the preparation method that the present invention provides the active sludge carbon of a kind of distiller grains that adulterate.The present invention adopts dirty mud as a raw material, and adulterate distiller grains, through microwave under anaerobic Fermented Condensed, and pyrolysis carbonization, through liquor zinci chloridi pretreatment, then high-temperature activation, dry with hydrochloric acid solution washing, it is thus achieved that inexpensive activated carbon.The present invention because of zinc chloride when low temperature to mud in Organic substance play dissolution, material is made to form original hole, and at high temperature there is certain catalytic dehydration and supporting role, there is provided a skeleton to when mud is by carbonization newborn carbon, newborn carbon has nascent key, there is absorption affinity, carbon and zinc chloride etc. can be made to combine, it is to avoid the generation of tar.After with hydrochloric acid solution the inorganic constituents such as zinc chloride being dissolved and cleaning, the surface of carbon is just exposed out becomes the active carbon pore structure with absorption affinity, is a kind of effectively make mud reach the method that resource stably utilizes.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
(1) take the mud that sewage treatment plants pressure filter is press-filtered out to mix with distiller grains 8:1 in mass ratio, in the environment that dissolved oxygen is 0.1 ~ 1.0mg/L, maintain the temperature at 35 ~ 37 DEG C, adding cyanophyceae, cyanophyceae and mixture quality ratio for 1:3, ferments 20 ~ 30 days, discharge biogas, filter, proceed to anaerobic tank and continue fermentation 30 ~ 40 days, filter, wash filtering residue 3 ~ 5 times with clear water, insert baking oven, dry, add pulverizer, be ground into 100 ~ 200 order powder, obtain charcoal concentration distiller grains sewage sludge powder；
(2) weigh 100 ~ 120 parts of above-mentioned distiller grains sewage sludge powder, insert in tube furnace, at 400 ~ 600 DEG C, pyrolysis carbonization 1h, obtain distiller grains mud carbide standby；
(3) take above-mentioned distiller grains mud carbide 50 ~ 60 parts to mix with 100 ~ 120 parts of 4mol/L liquor zinci chloridis, after stirring, impregnate 10 ~ 12h at normal temperatures, filter, air-dry, obtain dipping thing, standby；
(4) above-mentioned dipping thing being inserted baking oven after 100 ~ 110 DEG C of dry 10 ~ 12h, put into Muffle furnace, purge with carbon dioxide, carbon dioxide flow is 1 ~ 2L/min, and temperature is 400 ~ 700 DEG C, and constant temperature 1 ~ 2h is cooled to room temperature, obtains distiller grains active sludge carbon coarse fodder；
(5) take above-mentioned distiller grains active sludge carbon coarse fodder 3mol/L hydrochloric acid solution to clean, with 70 ~ 80 DEG C of deionized water wash to washing liquid in neutrality, obtain distiller grains active sludge carbon fines；
(6) take above-mentioned distiller grains active sludge carbon fines and insert baking oven in 100 ~ 110 DEG C of drying, be sized to 1 ~ 2.5mm, obtain distiller grains active sludge carbon.
The application process of the present invention is: it is 1mg/L ammonia nitrogen waste water that the distiller grains active sludge carbon 10g present invention prepared puts into 100mL concentration respectively, 100ml concentration is 100ug/L heavy metal chromium waste water, 100mL concentration is 100mg/L waste water from dyestuff, ammonia nitrogen removal frank is 75 ~ 84%, the clearance of chromium is 90 ~ 95%, and the clearance of TOC and colourity is 95 ~ 99%.
The method have the benefit that:
(1) present invention is with the excess sludge of sewage treatment plant and distiller grains slag for raw material, after a series of process, obtains distiller grains active sludge carbon, it is achieved the recycling to mud and distiller grains；
(2) the distiller grains active sludge carbon specific surface area of the preparation of the present invention is big, and ammonia nitrogen waste water, phosphorus-containing wastewater, heavy metal chromium waste water, waste water from dyestuff are had good eliminating rate of absorption；
(3) preparation method of the present invention is simple, with low cost.
Detailed description of the invention
Take the mud that sewage treatment plants pressure filter is press-filtered out to mix with distiller grains 8:1 in mass ratio, in the environment that dissolved oxygen is 0.1 ~ 1.0mg/L, maintain the temperature at 35 ~ 37 DEG C, adding cyanophyceae, cyanophyceae and mixture quality ratio for 1:3, ferments 20 ~ 30 days, discharge biogas, filter, proceed to anaerobic tank and continue fermentation 30 ~ 40 days, filter, wash filtering residue 3 ~ 5 times with clear water, insert baking oven, dry, add pulverizer, be ground into 100 ~ 200 order powder, obtain charcoal concentration distiller grains sewage sludge powder；Weigh 100 ~ 120 parts of above-mentioned distiller grains sewage sludge powder, insert in tube furnace, at 400 ~ 600 DEG C, pyrolysis carbonization 1h, obtain distiller grains mud carbide standby；Take above-mentioned distiller grains mud carbide 50 ~ 60 parts to mix with 100 ~ 120 parts of 4mol/L liquor zinci chloridis, after stirring, impregnate 10 ~ 12h at normal temperatures, filter, air-dry, obtain dipping thing, standby；Above-mentioned dipping thing being inserted baking oven after 100 ~ 110 DEG C of dry 10 ~ 12h, put into Muffle furnace, purge with carbon dioxide, carbon dioxide flow is 1 ~ 2L/min, and temperature is 400 ~ 700 DEG C, and constant temperature 1 ~ 2h is cooled to room temperature, obtains distiller grains active sludge carbon coarse fodder；Take above-mentioned distiller grains active sludge carbon coarse fodder 3mol/L hydrochloric acid solution to clean, with 70 ~ 80 DEG C of deionized water wash to washing liquid in neutrality, obtain distiller grains active sludge carbon fines；Take above-mentioned distiller grains active sludge carbon fines and insert baking oven in 100 ~ 110 DEG C of drying, be sized to 1 ~ 2.5mm, obtain distiller grains active sludge carbon.
Example 1
Take the mud that sewage treatment plants pressure filter is press-filtered out to mix with distiller grains 8:1 in mass ratio, in the environment that dissolved oxygen is 0.1mg/L, maintain the temperature at 35 DEG C, adding cyanophyceae, cyanophyceae and mixture quality ratio for 1:3, ferments 20 days, discharge biogas, filter, proceed to anaerobic tank and continue fermentation 30 days, filter, wash filtering residue 3 times with clear water, insert baking oven, dry, add pulverizer, be ground into 100 order powder, obtain charcoal concentration distiller grains sewage sludge powder；Weigh 100 parts of above-mentioned distiller grains sewage sludge powder, insert in tube furnace, in 400 DEG C of pyrolysis carbonization 1h, obtain distiller grains mud carbide standby；Take above-mentioned distiller grains mud carbide 50 parts to mix with 100 parts of 4mol/L liquor zinci chloridis, after stirring, impregnate 10h at normal temperatures, thing must be impregnated standby；Above-mentioned dipping thing being inserted baking oven after 100 DEG C of dry 10h, puts into Muffle furnace, purge with carbon dioxide, carbon dioxide flow is 1L/min, and temperature is 400 DEG C, and constant temperature 1h is cooled to room temperature, obtains distiller grains active sludge carbon coarse fodder standby；Take above-mentioned distiller grains active sludge carbon coarse fodder 3mol/L hydrochloric acid solution to clean, with 70 ~ 80 DEG C of deionized water wash to washing liquid in neutrality, obtain distiller grains active sludge carbon fines standby；Take above-mentioned distiller grains active sludge carbon fines and insert baking oven in 100 DEG C of drying, be sized to 2.5mm, obtain distiller grains active sludge carbon.
It is 1mg/L ammonia nitrogen waste water that the distiller grains active sludge carbon 10g present invention prepared puts into 100mL concentration respectively, 100mL concentration is 100ug/L heavy metal chromium waste water, and 100mL concentration is 100mg/L waste water from dyestuff, and ammonia nitrogen removal frank is 75%, the clearance of chromium is 90%, and the clearance of TOC and colourity is 95%.
Example 2
Take the mud that sewage treatment plants pressure filter is press-filtered out to mix with distiller grains 8:1 in mass ratio, in the environment that dissolved oxygen is 0.5mg/L, maintain the temperature at 36 DEG C, adding cyanophyceae, cyanophyceae and mixture quality ratio for 1:3, ferments 25 days, discharge biogas, filter, proceed to anaerobic tank and continue fermentation 35 days, filter, wash filtering residue 4 times with clear water, insert baking oven, dry, add pulverizer, be ground into 150 order powder, obtain charcoal concentration distiller grains sewage sludge powder；Weigh 110 parts of above-mentioned distiller grains sewage sludge powder, insert in tube furnace, in 500 DEG C of pyrolysis carbonization 1h, obtain distiller grains mud carbide standby；Take above-mentioned distiller grains mud carbide 55 parts to mix with 110 parts of 4mol/L liquor zinci chloridis, after stirring, impregnate 11h at normal temperatures, thing must be impregnated standby；Above-mentioned dipping thing being inserted baking oven after 105 DEG C of dry 11h, puts into Muffle furnace, purge with carbon dioxide, carbon dioxide flow is 1.5L/min, and temperature is 500 DEG C, and constant temperature 1.5h is cooled to room temperature, obtains distiller grains active sludge carbon coarse fodder standby；Take above-mentioned distiller grains active sludge carbon coarse fodder 3mol/L hydrochloric acid solution to clean, with 75 DEG C of deionized water wash to washing liquid in neutrality, obtain distiller grains active sludge carbon fines standby；Take above-mentioned distiller grains active sludge carbon fines and insert baking oven in 105 DEG C of drying, be sized to 2mm, obtain distiller grains active sludge carbon.
It is 1mg/L ammonia nitrogen waste water that the distiller grains active sludge carbon 10g present invention prepared puts into 100mL concentration respectively, 100mL concentration is 100ug/L heavy metal chromium waste water, and 100mL concentration is 100mg/L waste water from dyestuff, and ammonia nitrogen removal frank is 80%, the clearance of chromium is 92%, and the clearance of TOC and colourity is 97%.
Example 3
Take the mud that sewage treatment plants pressure filter is press-filtered out to mix with distiller grains 8:1 in mass ratio, in the environment that dissolved oxygen is 1.0mg/L, maintain the temperature at 37 DEG C, adding cyanophyceae, cyanophyceae and mixture quality ratio for 1:3, ferments 30 days, discharge biogas, filter, proceed to anaerobic tank and continue fermentation 40 days, filter, wash filtering residue 5 times with clear water, insert baking oven, dry, add pulverizer, be ground into 200 order powder, obtain charcoal concentration distiller grains sewage sludge powder；Weigh 120 parts of above-mentioned distiller grains sewage sludge powder, insert in tube furnace, in 600 DEG C of pyrolysis carbonization 1h, obtain distiller grains mud carbide standby；Take above-mentioned distiller grains mud carbide 60 parts to mix with 120 parts of 4mol/L liquor zinci chloridis, after stirring, impregnate 12h at normal temperatures, thing must be impregnated standby；Above-mentioned dipping thing being inserted baking oven after 110 DEG C of dry 12h, puts into Muffle furnace, purge with carbon dioxide, carbon dioxide flow is 2L/min, and temperature is 700 DEG C, and constant temperature 2h is cooled to room temperature, obtains distiller grains active sludge carbon coarse fodder standby；Take above-mentioned distiller grains active sludge carbon coarse fodder 3mol/L hydrochloric acid solution to clean, with 80 DEG C of deionized water wash to washing liquid in neutrality, obtain distiller grains active sludge carbon fines standby；Take above-mentioned distiller grains active sludge carbon fines and insert baking oven in 110 DEG C of drying, be sized to 1mm, obtain distiller grains active sludge carbon.
It is 1mg/L ammonia nitrogen waste water that the distiller grains active sludge carbon 10g present invention prepared puts into 100mL concentration respectively, 100mL concentration is 100ug/L heavy metal chromium waste water, and 100mL concentration is 100mg/L waste water from dyestuff, and ammonia nitrogen removal frank is 84%, the clearance of chromium is 95%, and the clearance of TOC and colourity is 99%.
Claims (1)
1. the preparation method of the distiller grains active sludge carbon that adulterates, it is characterised in that concrete preparation process is:
(1) take the mud that sewage treatment plants pressure filter is press-filtered out to mix with distiller grains 8:1 in mass ratio, in the environment that dissolved oxygen is 0.1 ~ 1.0mg/L, maintain the temperature at 35 ~ 37 DEG C, adding cyanophyceae, cyanophyceae and mixture quality ratio for 1:3, ferments 20 ~ 30 days, discharge biogas, filter, proceed to anaerobic tank and continue fermentation 30 ~ 40 days, filter, wash filtering residue 3 ~ 5 times with clear water, insert baking oven, dry, add pulverizer, be ground into 100 ~ 200 order powder, obtain charcoal concentration distiller grains sewage sludge powder；
(2) weigh 100 ~ 120 parts of above-mentioned distiller grains sewage sludge powder, insert in tube furnace, at 400 ~ 600 DEG C, pyrolysis carbonization 1h, obtain distiller grains mud carbide standby；
(3) take above-mentioned distiller grains mud carbide 50 ~ 60 parts to mix with 100 ~ 120 parts of 4mol/L liquor zinci chloridis, after stirring, impregnate 10 ~ 12h at normal temperatures, filter, air-dry, obtain dipping thing, standby；
(4) above-mentioned dipping thing being inserted baking oven after 100 ~ 110 DEG C of dry 10 ~ 12h, put into Muffle furnace, purge with carbon dioxide, carbon dioxide flow is 1 ~ 2L/min, and temperature is 400 ~ 700 DEG C, and constant temperature 1 ~ 2h is cooled to room temperature, obtains distiller grains active sludge carbon coarse fodder；
(5) take above-mentioned distiller grains active sludge carbon coarse fodder 3mol/L hydrochloric acid solution to clean, with 70 ~ 80 DEG C of deionized water wash to washing liquid in neutrality, obtain distiller grains active sludge carbon fines；
(6) take above-mentioned distiller grains active sludge carbon fines and insert baking oven in 100 ~ 110 DEG C of drying, be sized to 1 ~ 2.5mm, obtain distiller grains active sludge carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610306239.0A CN105776210A (en) | 2016-05-10 | 2016-05-10 | Preparation method of distillers'grain-doped sludge activated carbon |
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| CN201610306239.0A CN105776210A (en) | 2016-05-10 | 2016-05-10 | Preparation method of distillers'grain-doped sludge activated carbon |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500290A (en) * | 2017-10-16 | 2017-12-22 | 安徽工业大学 | Recycling treatment method of cassava alcohol sludge |
| CN110183257A (en) * | 2019-06-21 | 2019-08-30 | 中国科学院成都生物研究所 | A kind of complete utilization method of Maotai-flavor liquor distillage anaerobic digestion coupling hydrothermal carbonization |
| CN111994908A (en) * | 2020-08-11 | 2020-11-27 | 福建省热带作物科学研究所 | Preparation method of biomass charcoal for reducing nitrogen and phosphorus in soil |
| CN113666370A (en) * | 2021-09-27 | 2021-11-19 | 太原理工大学 | Method for preparing capacitance carbon material by secondary microbial fermentation and activation of vinasse |
| KR20210149993A (en) * | 2020-06-03 | 2021-12-10 | 한국세라믹기술원 | Manufacturing method of partially crystaline porous active carbon and super capacitor using the same and method of manufacturing thereof |
-
2016
- 2016-05-10 CN CN201610306239.0A patent/CN105776210A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500290A (en) * | 2017-10-16 | 2017-12-22 | 安徽工业大学 | Recycling treatment method of cassava alcohol sludge |
| CN110183257A (en) * | 2019-06-21 | 2019-08-30 | 中国科学院成都生物研究所 | A kind of complete utilization method of Maotai-flavor liquor distillage anaerobic digestion coupling hydrothermal carbonization |
| KR20210149993A (en) * | 2020-06-03 | 2021-12-10 | 한국세라믹기술원 | Manufacturing method of partially crystaline porous active carbon and super capacitor using the same and method of manufacturing thereof |
| KR102371851B1 (en) | 2020-06-03 | 2022-03-08 | 한국세라믹기술원 | Manufacturing method of partially crystaline porous active carbon and super capacitor using the same and method of manufacturing thereof |
| CN111994908A (en) * | 2020-08-11 | 2020-11-27 | 福建省热带作物科学研究所 | Preparation method of biomass charcoal for reducing nitrogen and phosphorus in soil |
| CN111994908B (en) * | 2020-08-11 | 2022-08-09 | 福建省热带作物科学研究所 | Preparation method of biomass charcoal for reducing nitrogen and phosphorus in soil |
| CN113666370A (en) * | 2021-09-27 | 2021-11-19 | 太原理工大学 | Method for preparing capacitance carbon material by secondary microbial fermentation and activation of vinasse |
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Application publication date: 20160720 |