CN108975336A - A kind of preparation method and application of oxygen-enriched active carbon - Google Patents

A kind of preparation method and application of oxygen-enriched active carbon Download PDF

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Publication number
CN108975336A
CN108975336A CN201811000024.1A CN201811000024A CN108975336A CN 108975336 A CN108975336 A CN 108975336A CN 201811000024 A CN201811000024 A CN 201811000024A CN 108975336 A CN108975336 A CN 108975336A
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China
Prior art keywords
active carbon
oxygen
enriched
preparation
water
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Pending
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CN201811000024.1A
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Chinese (zh)
Inventor
刘洪均
陈俊丰
龙云良
董平
曹晶晶
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Nanjing Aquacup Technology Co Ltd
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Nanjing Aquacup Technology Co Ltd
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Priority to CN201811000024.1A priority Critical patent/CN108975336A/en
Publication of CN108975336A publication Critical patent/CN108975336A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/354After-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

Abstract

The invention discloses a kind of preparation method and applications of oxygen-enriched active carbon, by porous activated carbon in strong acid, under conditions of the catalyst such as zinc nitrate/sodium nitrate, oxygen-enriched active carbon is prepared by the reaction of the combined oxidation of potassium permanganate and hydrogen peroxide, the reaction, which is made on the porous structure of active carbon, possesses a large amount of hydroxyl, carbonyl, the oxide-containing chemical group such as carboxyl, the oxygen-enriched active carbon can be directly assembled into active carbon filter core carry out using, simultaneously, modified powder active carbon can be prepared into molding carbon membrane, increase water body and passes through the runner in active carbon porous structure, efficiency is filtered out to heavy metal ion such as lead to further promote the modified activated carbon, it can be widely applied in all kinds of water purification installations and engineering of water treatment equipment.

Description

A kind of preparation method and application of oxygen-enriched active carbon
Technical field
The invention belongs to Water warfare fields, and in particular to a kind of preparation method and application of oxygen-enriched active carbon.
Background technique
China is mainly river, lake and reservoir as the surface water of drinking water source, is divided the monitoring of this few class water body Analysis shows that these surface water have received the pollution of the heavy metals such as lead, cadmium.Heavy metal is easily biological by food chain Enrichment is constituted and is seriously threatened to biology and human health.The pollution of source water not only give biology and human health bring compared with Big harm, and make a big impact to the traditional water-purifying process in waterworks and water quality.Not with people's living standard It is disconnected to improve, the progress of means is tested and analyzed, requirement of the people to drinking water quality will be more stringent, corresponding water supply quality standard Also it is being continuously improved.Therefore, the heavy metal how being effectively removed in drinking water, it has also become when next environment urgently to be solved Problem.
With heavy metal existing for various chemical states or chemical form, will be retained after entering environment or the ecosystem, Accumulation and migration, cause damages.Such as: lead is that a kind of distribution is wide, has accumulative environmental contaminants, and it is pair that property, which is stablized, The highly unwanted heavy metal element of human body, while also seriously endangering the health of children.With the rapid hair of industry and other industry Exhibition, a large amount of uses of lead, lead contamination are extended from occupational environment to water, atmosphere, food, medicine and everyday environments, because This has become the pressing problem that each field is faced except lead.
Wherein, the lead in waste water is mainly from the exploitation of lead ore, smelting and industrial discharge, motor vehicle exhaust emission It can cause water pollution.When lead concentration reaches 0.1mg/L in water, the self purification of water body, Drinking Water national standard will be inhibited Provide that lead content must not be higher than 0.01mg/L, and lead content is significantly larger than standard in sewage, therefore water process is removed lead technology and had become For research emphasis.The chemical method of conventional process lead mainly has: the precipitation method, coacervation, absorption method, ion-exchange, reverse osmosis Method etc..
In water purification industry, current conventional processing method is osmosis filtration method, and reverse osmosis water purification machine is for heavy metal (including lead) to filter out effect very good, but it wastes water very much, and reverse osmosis technology is produced along with a large amount of discharge of wastewater 1 liter of pure water needs to exhaust the waste water (different depending on use environment and temperature) of 3-8 liter, can substitute reverse osmosis purified water technology It is novel that filter out heavy metal technical need strong.
Active carbon can effectively remove organic matter, chlorine residue, radioactive substance in water, and have decoloration, remove odors and other effects, Its standard configuration for having been considered as water purification product.The present common active carbon filter core of water purification industry have bulk active filtration core and Constitutive active carbon rod filter core two major classes.However to filter out heavy metal (lead) efficiency lower for current active carbon, needs to carry out depth and opens Hair promotes it except lead effect.
The characterization of adsorption of active carbon depends not only on its pore structure, and depends on its surface chemical property, compares table Area and pore structure influence the adsorption capacity of active carbon, and surface chemical property affects active carbon same polarity or nonpolarity is inhaled Interaction force between attached matter.The main component of active carbon itself is carbon, itself does not have polarity, is in hydrophobicity, but carbon materials Expect oxidizing by oxygen gas and water etc. in air and generate the functional groups such as a small amount of carbonyl, carboxyl, hydroxyl, to improve Active carbon to the adsorptions of polar substances, but on the whole its to heavy metal to filter out efficiency still lower.
Summary of the invention
Aiming at the existing problems and shortcomings of the prior art, the technical problem to be solved by the invention is to provide a kind of oxygen-enriched The preparation method and application of active carbon, the molding carbon membrane being prepared by this method is while realizing physical filtering, to a huge sum of money Belong to lead ion with efficiently efficiency is filtered out, can be widely applied in all kinds of water purification installations and engineering of water treatment equipment.
In order to achieve the above object, first aspect present invention the technical solution adopted is as follows:
A kind of preparation method of oxygen-enriched active carbon, which comprises the steps of:
(1) with composite catalyst, active carbon is pre-oxidized by potassium permanganate under cryogenic, adjusts pH value of solution Value, then by heating water bath, is stirred to react;
(2) reactive bath technique of step (1) is cooling, combined oxidation is carried out, is stirred to react and stops after a certain period of time, to make to live Property carbon surface forms a large amount of hydroxyl, carbonyl and carboxylic group;
(3) product after step (2) oxidation is filtered and is washed repeatedly with HCl solution and deionized water until nothing in filtrate Until sulfate radical is detected, charcoal cake is filtered to obtain, filter cake is placed in the vacuum oven of certain temperature and is sufficiently dried, to obtain Obtain oxygen-enriched active carbon.
It is further limited as of the invention, in the preparation method step (1), the composite catalyst is certain matter The concentrated sulfuric acid and zinc nitrate of amount or the concentrated sulfuric acid and sodium nitrate of certain mass.
It is further limited as of the invention, in the preparation method step (1), the cryogenic conditions are 10 DEG C of ice water Bath, the solution ph are 1, and the temperature of the heating water bath is 45 DEG C~100 DEG C, and being stirred to react the time is 1h~12hrs.
It is further limited as of the invention, in the preparation method step (2), temperature that the reactive bath technique is cooled to It is 0~20 DEG C, carrying out reagent used in combined oxidation is hydrogen peroxide, and the time being stirred to react is 30min~2hrs.
It is further limited as of the invention, in the preparation method step (3), the HCl solution is that 5%HCl is molten Liquid, the temperature of the vacuum oven are set as 45 DEG C~80 DEG C.
The second aspect of the invention provides the application of oxygen-enriched active carbon made from first aspect according to the present invention, should Oxygen-enriched active carbon made from method can be directly assembled into active carbon filter core carry out using, meanwhile, can be by modified powder active carbon It is prepared into molding carbon membrane, increases water body by the runner in active carbon porous structure, to further promote modification work Property charcoal can be widely applied in all kinds of water purification installations and engineering of water treatment equipment the efficiency that filters out of the heavy metal ion such as lead.
Technical solution of the present invention has the following advantages that and advantageous effects:
1, the oxygen-enriched active carbon of method preparation of the invention, while realizing physical filtering, can be obviously improved its to Lead ion is the removal of heavy metal ions efficiency of representative, comprehensive decontamination water quality.
2, the oxygen-enriched active carbon of method of the invention preparation will be in active carbon by the preparation process route of Strong oxdiative Porous surface prepares a large amount of carbonyl, carboxyl, hydroxy functional group, imitates to promote modified activated carbon to the removal of land pollutant Energy.
3, the oxygen-enriched active carbon of method preparation of the invention, can be directly assembled into active carbon filter core carry out using, meanwhile, Modified powder active carbon can be prepared into molding carbon membrane, increase water body by the runner in active carbon porous structure, thus into The promotion of the one step modified activated carbon filters out efficiency to heavy metal ion such as lead.
4, the oxygen-enriched active carbon of method of the invention preparation, can be widely applied to all kinds of water purification installations and engineering of water treatment In equipment.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes part of this application, not Inappropriate limitation of the present invention is constituted, in the accompanying drawings:
Fig. 1 is the preparation technology flow chart of the oxygen-enriched active carbon of the present invention.
Specific embodiment
It will come that the present invention will be described in detail with following specific embodiment below, illustrative examples of the invention and say herein It is bright to be used to explain the present invention but not as a limitation of the invention.
Embodiment 1:
The preparation of oxygen-enriched active carbon:
(10 DEG C) assemble the reaction flask of 1L in ice-water bath, and deionized water 500ml is added, adds high potassium permanganate 6g is added 1 gram of sodium nitrate, adds the concentrated sulfuric acid, adjusts pH value to 1, adds granular activated carbon 300g (12~24 mesh), gradually Bath temperature is risen to 45 degree, is stirred to react 1 hour;Reactive bath technique is then cooled to 20 DEG C, adds hydrogen peroxide 5ml, is stirred Stop after reaction 30min.
Reaction solution is filtered while hot, 5%HCl solution and deionized water are washed until sulfate radical-free is detected to be in filtrate Only, finally filter cake is placed in 60 DEG C of vacuum oven and is sufficiently dried, oxygen-enriched active carbon is made.
Embodiment 2:
Oxygen-enriched active carbon is evaluated and tested except lead effect
It takes 2 UDF filter cores (size: 10 cun of standard), and difference label A (granular activated carbon of conventional 12~24 mesh, 240 Gram), B (the oxygen-enriched active carbon prepared by case study on implementation 1,240 grams).The lead concentration of configuration challenge liquid 100ppb challenges water, Under the pressure of 0.2bar, the lead of test UDF filter core A, B remove efficiency, and survey water inventory is 5000L.
It is clearly showed that by data, the more common active carbon filter core of oxygen enrichment active carbon filter core has removing by a relatively large margin Lead performance boost.
Table one: active carbon filter core removes lead experimental data.
Flow (L) A B
10 20% 95%
1000 16% 95%
2000 10% 94%
3000 8% 91%
4000 5% 88%
5000 0 85%
Embodiment 3:
The chlorine residue removal efficiency evaluation and test of oxygen-enriched active carbon
The challenge water that contents of residual chlorine is 2.0ppm is configured, under the pressure of 0.2bar, is tested UDF (size: 10 cun of standard) Filter core A (granular activated carbon of conventional 12~24 mesh, 240 grams), B (the feeding active carbon of richness prepared by case study on implementation 1,240 grams) Chlorine residue removal efficiency (test condition: chlorine residue spiked levels 2ppm, test pressure 2ba), surveys water inventory be 5000L.
Table one: active carbon filter core removes chlorine residue experimental data
Flow (L) A B
10 96% 95%
1000 94% 91%
2000 90% 85%
3000 85% 78%
4000 75% 69%
5000 62% 55%
It can be seen that, active carbon UDF filter core A and B present preferable chlorine residue removal efficiency from above-mentioned experimental data, can It is used suitable for extensive water purification product;But under the chlorine residue adsorption of the oxygen-enriched more regular activated filtration core A of active carbon filter core B Drop comparatively fast, possible reason is to destroy the surface texture of a part of active carbon in the preparation process of oxygen-enriched active carbon, from And the chlorine residue adsorption for reducing active carbon to a certain extent.
It is provided for the embodiments of the invention technical solution above to be described in detail, applies specific case pair herein The principle and embodiment of the embodiment of the present invention are expounded, and the explanation of above embodiments is only applicable to help to understand this hair Bright principle;At the same time, for those skilled in the art in specific embodiment and is answered according to embodiments of the present invention With in range, there will be changes, in conclusion the contents of this specification are not to be construed as limiting the invention.

Claims (6)

1. a kind of preparation method of oxygen-enriched active carbon, which comprises the steps of:
(1) with composite catalyst, active carbon is pre-oxidized by potassium permanganate under cryogenic, adjusts solution ph, Then it by heating water bath, is stirred to react;
(2) reactive bath technique of step (1) is cooling, combined oxidation is carried out, is stirred to react and stops after a certain period of time, to make active carbon Surface forms a large amount of hydroxyl, carbonyl and carboxylic group;
(3) by step (2) oxidation after product filtering and with HCl solution and deionized water wash repeatedly until in filtrate without sulfuric acid Until root is detected, charcoal cake is filtered to obtain, filter cake is placed in the vacuum oven of certain temperature and is sufficiently dried, to obtain richness Oxygen activity charcoal.
2. the preparation method of oxygen-enriched active carbon according to claim 1, which is characterized in that the composite catalyst is certain The concentrated sulfuric acid and zinc nitrate of quality or the concentrated sulfuric acid and sodium nitrate of certain mass.
3. the preparation method of oxygen-enriched active carbon according to claim 1, which is characterized in that the cryogenic conditions are 10 DEG C of ice Water-bath, the solution ph are 1, and the temperature of the heating water bath is 45 DEG C~100 DEG C, and being stirred to react the time is 1h~12hrs.
4. the preparation method of oxygen-enriched active carbon according to claim 1, which is characterized in that the temperature that the reactive bath technique is cooled to Degree is 0~20 DEG C, and carrying out reagent used in combined oxidation is hydrogen peroxide, and the time being stirred to react is 30min~2hrs.
5. the preparation method of oxygen-enriched active carbon according to claim 1, which is characterized in that the HCl solution is 5%HCl Solution, the temperature of the vacuum oven are set as 45 DEG C~80 DEG C.
6. the application of oxygen-enriched active carbon, which is characterized in that, can according to oxygen-enriched active carbon made from any one of Claims 1 to 5 Be directly assembled into active carbon filter core carry out using, meanwhile, modified powder active carbon can be prepared into molding carbon membrane, increase water Body filters out the heavy metal ion such as lead to further promote the modified activated carbon by the runner in active carbon porous structure Effect can be widely applied in all kinds of water purification installations and engineering of water treatment equipment.
CN201811000024.1A 2018-08-20 2018-08-20 A kind of preparation method and application of oxygen-enriched active carbon Pending CN108975336A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110813235A (en) * 2019-11-21 2020-02-21 安徽工业大学 Nickel ion adsorbent and preparation method thereof
CN110975804A (en) * 2019-11-21 2020-04-10 安徽工业大学 Zinc ion adsorbent and preparation method thereof
CN111249765A (en) * 2020-02-25 2020-06-09 中国科学院化学研究所 Pressurized fluid extraction system and method for removing metal ions from carbon material
CN115105949A (en) * 2022-07-08 2022-09-27 潮州市索力德机电设备有限公司 Method for reducing NOx emission of ceramic gas tunnel kiln

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CN1087878A (en) * 1992-12-10 1994-06-15 王宝贞 The efficient process for purifying water that removes radioactivity and heavy metal
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CN102284304A (en) * 2009-12-31 2011-12-21 中国科学院成都有机化学有限公司 Method for preparing high-efficiency catalyst for vinyl acetate synthesis by acetylene method
CN106082214A (en) * 2016-06-22 2016-11-09 宁夏医科大学 Load MnO2radix Astragali waste residue activated carbon and preparation method thereof
CN106512944A (en) * 2016-12-06 2017-03-22 福建师范大学 Production method of oxidized wood active carbon for effectively adsorbing carbon dioxide

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* Cited by examiner, † Cited by third party
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US4831011A (en) * 1986-02-17 1989-05-16 Nippondenso Co., Ltd. Carbon-based adsorbent and process for production thereof
CN1087878A (en) * 1992-12-10 1994-06-15 王宝贞 The efficient process for purifying water that removes radioactivity and heavy metal
CN1513777A (en) * 2003-03-17 2004-07-21 哈尔滨工业大学 Permangnate preoxidation and bioactive carbon combined use to remove contamination technique
CN102284304A (en) * 2009-12-31 2011-12-21 中国科学院成都有机化学有限公司 Method for preparing high-efficiency catalyst for vinyl acetate synthesis by acetylene method
CN106082214A (en) * 2016-06-22 2016-11-09 宁夏医科大学 Load MnO2radix Astragali waste residue activated carbon and preparation method thereof
CN106512944A (en) * 2016-12-06 2017-03-22 福建师范大学 Production method of oxidized wood active carbon for effectively adsorbing carbon dioxide

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110813235A (en) * 2019-11-21 2020-02-21 安徽工业大学 Nickel ion adsorbent and preparation method thereof
CN110975804A (en) * 2019-11-21 2020-04-10 安徽工业大学 Zinc ion adsorbent and preparation method thereof
CN111249765A (en) * 2020-02-25 2020-06-09 中国科学院化学研究所 Pressurized fluid extraction system and method for removing metal ions from carbon material
CN111249765B (en) * 2020-02-25 2021-04-06 中国科学院化学研究所 Pressurized fluid extraction system and method for removing metal ions from carbon material
CN115105949A (en) * 2022-07-08 2022-09-27 潮州市索力德机电设备有限公司 Method for reducing NOx emission of ceramic gas tunnel kiln
CN115105949B (en) * 2022-07-08 2023-08-11 潮州市索力德机电设备有限公司 Method for reducing NOx discharged by ceramic gas tunnel kiln

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Application publication date: 20181211