CN108373248A - A method of quickly preparing porous magnetic activated coke based on dewatered sludge - Google Patents
A method of quickly preparing porous magnetic activated coke based on dewatered sludge Download PDFInfo
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- CN108373248A CN108373248A CN201810103964.7A CN201810103964A CN108373248A CN 108373248 A CN108373248 A CN 108373248A CN 201810103964 A CN201810103964 A CN 201810103964A CN 108373248 A CN108373248 A CN 108373248A
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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
- C02F11/00—Treatment of sludge; Devices therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01J20/28002—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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- 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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L5/00—Solid fuels
- C10L5/40—Solid fuels essentially based on materials of non-mineral origin
- C10L5/46—Solid fuels essentially based on materials of non-mineral origin on sewage, house, or town refuse
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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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
- C02F2303/00—Specific treatment goals
- C02F2303/06—Sludge reduction, e.g. by lysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Environmental & Geological Engineering (AREA)
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- Hydrology & Water Resources (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
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Abstract
The present invention provides a kind of methods quickly preparing porous magnetic activated coke based on dewatered sludge, and dewatered sludge is air-dried, mud granule is ground into；Mud granule after drying is put into stainless steel cauldron, distilled water, sealing is added, magnetic agitation is reacted after heating；After reaction, cooling, cleaning, vacuum filter, obtain forerunner's product；Forerunner's product is immersed in activator and catalyst solution, sealed soak oscillation, vacuum filter heats after being air-dried, reaction；Then cooling, cleaning, drying are to get porous magnetic activated coke.Present invention process process is simple, quick, safety is good, reaction is mild, low energy consumption, and gained activated coke pore structure is flourishing, has good magnetism, it is easily recycled and carries out regeneration recycling, it can be widely applied in waste water and waste gas pollution control and treatment, expanded recycling sludge significantly and utilized field, there is significant economic benefit and environmental benefit.
Description
Technical field
The invention belongs to changing rejected material to useful resource technical field, more particularly to one kind quickly preparing porous magnetic based on dewatered sludge
The method of property activated coke.
Background technology
According to statistics, China's municipal sewage treatment excess sludge production in 2016 is up to 43,000,000 tons (moisture content 80%), existing
Stage main processing method includes aerobic/anaerobic digestion, dehydration and drying burning and sanitary landfills etc..However, China's sludge
Yield is huge, processing capacity wretched insufficiency at this stage, therefore the safe handling of sludge has become China with disposition and is badly in need of solving
One of environmental problem certainly directly affects ecological environment security and health.
In recent years, have it is more for sewage disposal excess sludge is innoxious and minimizing in terms of research and application, such as
Sludge anaerobic/aerobic sigestion, heat chemistry hydrolysis, ultrasonic disintegration, microwave treatment, high-level oxidation technology etc., but about sludge resource
Change relatively fewer using the research of technical aspect.Applicant seminar early period using hydrothermal carbonization technology to biological sludge dehydration and
Minimizing efficiency is studied, it is found that it is the utilization approaches with feasibility to convert biological sludge to hydro-thermal coke,
Calorific value can be used as derived solid fuel and utilized (patent authorization number up to 15-18MJ/kg：ZL 201410143389.5).
Nevertheless, since its specific surface area is smaller, it is difficult in being handled for heavy metal and organic polluting water as adsorbent, to
Limit its recycling range.Therefore, it studies and expands recycling sludge and utilize field, exploitation is quick, low consumption, easily recycles
Porous structure magnetism activated coke technology of preparing, the promotion of sludge reduction and recycling added value is of great significance and is answered
With value.
Invention content
The technical problem to be solved by the present invention is to how prepare the magnetic activated coke of pore structure prosperity.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is to provide one kind, and based on dewatered sludge, quickly preparation is more
The method of hole magnetism activated coke, which is characterized in that step is：
Step 1：Dewatered sludge is air-dried, mud granule is ground into；Mud granule after drying is put into stainless steel
In reaction kettle, distilled water, sealing is added, magnetic agitation is reacted after heating；After reaction, cooling, cleaning, vacuum filter, obtain
To forerunner's product；
Step 2：Forerunner's product prepared by step 1 immerses in activator and catalyst solution, sealed soak oscillation, vacuum
Filtering is heated after being air-dried, reaction；Then cooling, cleaning, drying are to get porous magnetic activated coke.
Preferably, in the step 1, dewatered sludge moisture content is 60%-80%.
Preferably, in the step 1, a diameter of 1-3mm of mud granule.
Preferably, in the step 1, the mass ratio of dewatered sludge and distilled water is 0.2-3.0.
Preferably, in the step 1, magnetic agitation speed 500-800r/min.
Preferably, in the step 1,0.5-2h is reacted after being heated to 160-260 DEG C.
Preferably, in the step 1, cleaning includes hydrochloric acid flushing, ethyl alcohol or acetone soak, distilled water flushing, wherein salt
Acid concentration is 0.1-0.5mol/L, and ethyl alcohol or acetone volume fraction are 50%-85%.
Preferably, in the step 2, activator is zinc chloride, potassium hydroxide, potassium carbonate, phosphoric acid or sodium dihydrogen phosphate；It is living
The mass ratio of agent and dewatered sludge is 0.05-0.20.
Preferably, in the step 2, catalyst is hydrogen in statu nascendi iron oxide or ferrous hydroxide；Catalyst and dehydration are dirty
The mass ratio of mud is 0.1-0.5.
Preferably, in the step 2, sealed soak vibrates 2-8h, oscillation rate 100-300r/min；Through being air-dried
Afterwards 30-120min is reacted at 500-700 DEG C.
Magnetic activated coke prepared by the present invention can be used as waste water and waste gas pollution control and treatment adsorbent, advanced oxidation free radical to swash
Agent living and solid fuel are applied.
Compared with prior art, the present invention has the advantages that：
(1) process of preparing of the present invention is simple and quick, and safety is good, and reaction is mild, and low energy consumption, gained activated coke hole
Structure is flourishing, has good magnetism, overcomes the defect that hydro-thermal coke ratio surface area and pore volume are small obtained by single hydrothermal carbonization,
And be easily recycled and carry out regeneration recycling, it can be widely applied in waste water and waste gas pollution control and treatment.
(2) present invention utilizes special physico-chemical property and solvation effect of the distilled water under subcritical state, realizes to dirt
The carbonization of mud and forming process, not only energy consumption is lower than conventional pyrolytic process, but also can greatly shorten the reaction time.
(3) sludge can not only be carried out innoxious and minimizing processing by the present invention, can also obtain pore structure prosperity
Magnetic activated coke, expanded significantly recycling sludge utilize field, have significant economic benefit and environmental benefit.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.
Embodiment 1
The dewatered sludge that moisture content is 80% is air-dried, the particle that diameter is about 1mm is ground into, 5g is taken to be put into
Volume is that 5mL distilled water, sealing is added in the stainless steel cauldron of 100mL, and control magnetic stirring speed is 500r/min, is added
Heat is to 160 DEG C of reaction 0.5h, after reaction, by reaction kettle cooled to room temperature, pours out the solidliquid mixture of reaction gained
It in beaker, is rinsed using a concentration of 0.1mol/L hydrochloric acid of 10mL, then the ethyl alcohol for being 85% with 10mL volume fractions impregnates, then
Using 50mL distilled water flushings, vacuum filter obtains 2.9g forerunner's product after finally weighing.
Forerunner's product of the above-mentioned gained of 2.5g is weighed in the conical flask equipped with 50mL distilled water, is then respectively adding 0.5g
Hydrogen in statu nascendi iron oxide and 0.25g zinc chloride, sealing impregnate oscillation 2h, then vacuum filter, through sky under 100r/min rates
30min is reacted at 500 DEG C after gas drying, is cooled to room temperature, uses a concentration of 0.1mol/L hydrochloric acid of 10mL and 10mL distilled water
It rinses, is then dried for 24 hours to get porous magnetic activated coke at 105 DEG C.After measured, which is 14.6MJ/kg,
Specific surface area is 167m2/ g, saturation magnetization 6.58emu/g, can to the saturated extent of adsorption of tetracycline antibiotic in water
Up to 52.7mg/g.
Embodiment 2
The dewatered sludge that moisture content is 60% is air-dried, the particle that diameter is about 3mm is ground into, 10g is taken to put
Entering in the stainless steel cauldron that volume is 100mL, 20mL distilled water, sealing is added, control magnetic stirring speed is 800r/min,
260 DEG C of reaction 2h are heated to, after reaction, by reaction kettle cooled to room temperature, pour out the solidliquid mixture of reaction gained
In beaker, rinsed using a concentration of 0.1mol/L hydrochloric acid of 20mL, then the acetone soak for being 50% with 20mL volume fractions, then
Using 40mL distilled water flushings, vacuum filter obtains 4.5g forerunner's product after finally weighing.
Forerunner's product of the above-mentioned gained of 2.5g is weighed in the conical flask equipped with 50mL distilled water, is then respectively adding
0.25g hydrogen in statu nascendi ferrous oxide and 0.75g potassium hydroxide, sealing impregnate oscillation 8h, then vacuum under 300r/min rates
Filtering, reacts 120min at 700 DEG C after being air-dried, is cooled to room temperature, using a concentration of 0.1mol/L hydrochloric acid of 10mL and
Then 10mL distilled water flushings are dried at 105 DEG C for 24 hours to get porous magnetic activated coke.After measured, which is
18.6MJ/kg, specific surface area 421m2/ g, saturation magnetization 7.08emu/g satisfy to tetracycline antibiotic in water
With adsorbance up to 98.4mg/g.
The above, only presently preferred embodiments of the present invention, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, can also make
Several improvement and supplement, these are improved and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, when made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution of any equivalent variations made by above-described embodiment, still fall within the range of technical scheme of the present invention
It is interior.
Claims (10)
1. a kind of method quickly preparing porous magnetic activated coke based on dewatered sludge, which is characterized in that step is：
Step 1：Dewatered sludge is air-dried, mud granule is ground into；Mud granule after drying is put into stainless steel reaction
In kettle, distilled water, sealing is added, magnetic agitation is reacted after heating；After reaction, cooling, cleaning, vacuum filter, before obtaining
Drive product；
Step 2：Forerunner's product prepared by step 1 immerses in activator and catalyst solution, sealed soak oscillation, vacuum mistake
Filter is heated after being air-dried, reaction；Then cooling, cleaning, drying are to get porous magnetic activated coke.
2. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 1, dewatered sludge moisture content is 60%-80%.
3. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 1, a diameter of 1-3mm of mud granule.
4. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 1, the mass ratio of dewatered sludge and distilled water is 0.2-3.0.
5. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 1, magnetic agitation speed 500-800r/min.
6. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 1,0.5-2h is reacted after being heated to 160-260 DEG C.
7. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 1, cleaning includes hydrochloric acid flushing, ethyl alcohol or acetone soak, distilled water flushing, and wherein concentration of hydrochloric acid is 0.1-
0.5mol/L, ethyl alcohol or acetone volume fraction are 50%-85%.
8. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 2, activator is zinc chloride, potassium hydroxide, potassium carbonate, phosphoric acid or sodium dihydrogen phosphate；Activator is dirty with dehydration
The mass ratio of mud is 0.05-0.20.
9. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 2, catalyst is hydrogen in statu nascendi iron oxide or ferrous hydroxide；The mass ratio of catalyst and dewatered sludge is
0.1-0.5。
10. a kind of method quickly being prepared porous magnetic activated coke based on dewatered sludge as described in claim 1, feature are existed
In：In the step 2, sealed soak vibrates 2-8h, oscillation rate 100-300r/min；In 500-700 after being air-dried
30-120min is reacted at DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876770A (en) * | 2019-03-13 | 2019-06-14 | 重庆大学 | The preparation method and application of magnetic hydro-thermal carbon adsorbent |
| CN110577219A (en) * | 2019-09-29 | 2019-12-17 | 南京工程学院 | Magnetic sludge straw-based activated carbon and preparation method thereof |
| CN113251422A (en) * | 2021-06-21 | 2021-08-13 | 中国环境科学研究院 | Non-pollution low-energy-consumption garbage recycling treatment method and system |
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| CN103521180A (en) * | 2013-09-29 | 2014-01-22 | 福建工程学院 | Method for preparing sludge-based formed magnetic active carbon |
| KR20150001001A (en) * | 2013-06-26 | 2015-01-06 | 대전대학교 산학협력단 | Adsorption Characteristics of H2S on Adsorbent Made by Drinking Water Treatment Sludge |
| CN106744952A (en) * | 2016-11-29 | 2017-05-31 | 中冶华天南京工程技术有限公司 | The method that sewage sludge prepares modified active coke |
| CN107572524A (en) * | 2017-09-15 | 2018-01-12 | 华中科技大学 | A kind of method that activated carbon is prepared using sludge |
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2018
- 2018-02-01 CN CN201810103964.7A patent/CN108373248B/en active Active
Patent Citations (4)
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| KR20150001001A (en) * | 2013-06-26 | 2015-01-06 | 대전대학교 산학협력단 | Adsorption Characteristics of H2S on Adsorbent Made by Drinking Water Treatment Sludge |
| CN103521180A (en) * | 2013-09-29 | 2014-01-22 | 福建工程学院 | Method for preparing sludge-based formed magnetic active carbon |
| CN106744952A (en) * | 2016-11-29 | 2017-05-31 | 中冶华天南京工程技术有限公司 | The method that sewage sludge prepares modified active coke |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876770A (en) * | 2019-03-13 | 2019-06-14 | 重庆大学 | The preparation method and application of magnetic hydro-thermal carbon adsorbent |
| CN110577219A (en) * | 2019-09-29 | 2019-12-17 | 南京工程学院 | Magnetic sludge straw-based activated carbon and preparation method thereof |
| CN113251422A (en) * | 2021-06-21 | 2021-08-13 | 中国环境科学研究院 | Non-pollution low-energy-consumption garbage recycling treatment method and system |
| CN113251422B (en) * | 2021-06-21 | 2022-02-15 | 中国环境科学研究院 | Non-pollution low-energy-consumption garbage recycling treatment method and system |
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