CN106362687A - Sepiolite adsorbent as well as preparation method and regeneration method thereof - Google Patents
Sepiolite adsorbent as well as preparation method and regeneration method thereof Download PDFInfo
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- 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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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
- B01J20/3244—Non-macromolecular compounds
- B01J20/3246—Non-macromolecular compounds having a well defined chemical structure
- B01J20/3248—Non-macromolecular compounds having a well defined chemical structure the functional group or the linking, spacer or anchoring group as a whole comprising at least one type of heteroatom selected from a nitrogen, oxygen or sulfur, these atoms not being part of the carrier as such
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
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- B01J20/34—Regenerating or reactivating
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- 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
- C02F2303/00—Specific treatment goals
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Abstract
The invention discloses a preparation method of a sepiolite adsorbent. The preparation method of the sepiolite adsorbent comprises the following steps: acidizing sepiolite, then washing the sepiolite with water until the sepiolite is neutral, and drying the sepiolite to obtain preprotreated sepiolite; adding an organic solution into the preprotreated sepiolite, steeping the preprotreated sepiolite, performing filtration, water washing, drying and grinding after steeping is finished, then introducing nitrogen, and performing activation at a temperature of 300-600 DEG C, thereby obtaining modified sepiolite; mixing the modified sepiolite with semi coke in proportion, thereby obtaining the sepiolite adsorbent. The sepiolite adsorbent prepared by the preparation method of the sepiolite adsorbent, provided by the invention, has the characteristics of good adsorption property and low cost; a regeneration method of the adsorbent is simple and low in regeneration energy consumption; based on the preparation method of the sepiolite adsorbent, the invention also provides the sepiolite adsorbent and the regeneration method of the sepiolite adsorbent.
Description
Technical field
The present invention relates to technical field of waste water processing and in particular to a kind of meerschaum adsorbent and preparation method thereof, regeneration
Method.
Background technology
Water is that the mankind depend on for existence and development indispensable resource, with China's expanding economy, urbanization and industry
The propulsion changed result in serious water pollution, the variety classes that particularly industry such as printing and dyeing, pharmacy, process hides and chemical industry is brought
Waste water.
In method of wastewater treatment, absorption method, as simple, the lower-cost method of one kind, widely should obtain
With.In correlation technique, common adsorbent is usually acticarbon or metal, the nonmetallic oxidation with carbonaceous as raw material
Species adsorbent, wherein acticarbon adsorption effect are preferable but relatively costly, and metal, nonmetal oxide class adsorbent are then
Absorbability is relatively low.And in correlation technique, different types of waste water needs to be adsorbed with different types of adsorbent, adsorbent
Range of application narrow.
Therefore, it is necessary to provide that a kind of absorption property is good, the adsorbent of low cost and applied range solves above-mentioned technology
Problem.
Content of the invention
The purpose of the present invention is to overcome above-mentioned technical problem, provides a kind of preparation method of meerschaum adsorbent, is prepared into
To meerschaum adsorbent have the characteristics that absorption property is good, low cost；And the renovation process of this adsorbent is simple, regeneration energy consumption
Low.
Technical scheme is as follows:
A kind of preparation method of meerschaum adsorbent, comprises the steps:
Meerschaum pretreatment: be washed to neutrality by after meerschaum acidification, and be dried to obtain pretreatment meerschaum；
Meerschaum is modified: adds organic solution to be impregnated in described pretreatment meerschaum, carried out after the completion of dipping
Filter, washing, drying, grinding, then pass to nitrogen and are activated under the conditions of 300-600 DEG C, obtain modified meerschaum；
Adsorbent is prepared: modified meerschaum is mixed in proportion with semi-coke, obtains meerschaum adsorbent.
Preferably, in described meerschaum modification procedure, organic solution is dodecylbenzene sodium sulfonate or cetyl front three
Base ammonium bromide, the concentration of described organic solution is 1-10mmol/l.
Preferably, in described meerschaum modification procedure, soak time is 30-180min.
Preferably, in described meerschaum pretreatment step, acid solution used by meerschaum acidification technique be nitric acid or
Hydrochloric acid, solubility is 0.2-1.5mol/l.
Preferably, meerschaum and the mass ratio of acid solution are 1:5-20.
Preferably, in described meerschaum pretreatment step, baking temperature is 100-120 DEG C.
Preferably, in described adsorbent preparation steps, modified meerschaum is 1:0.1-10 with the mass ratio of semi-coke.
Preferably, in described adsorbent preparation steps, the granularity of described modified meerschaum is 12-180 mesh, described semi-coke
Granularity is 80-140 mesh.
Based on the preparation method of described meerschaum adsorbent, the present invention also provides a kind of system by described meerschaum adsorbent
The meerschaum adsorbent that Preparation Method prepares.
The present invention also provides a kind of renovation process of meerschaum adsorbent, comprising: be used for inhaling by described meerschaum adsorbent
After attached waste water, in the adsorbent be adsorbed with waste, it is passed through air, and is heated to 300-600 DEG C and carry out Regeneration Treatment, obtain again
Raw meerschaum adsorbent.
Meerschaum adsorbent providing compared to prior art, the present invention and preparation method thereof, renovation process beneficial effect
It is:
First, the preparation method of the meerschaum adsorbent that the present invention provides, with the meerschaum of loose structure and semi-coke as raw material,
The meerschaum adsorbent absorption property obtaining is excellent；By adjusting the ratio of meerschaum and semi-coke, can be applicable to different types of useless
Water process, thus improve its range of application；
2nd, the meerschaum adsorbent that the present invention provides, with the meerschaum of loose structure and semi-coke as raw material, with low cost.
3rd, the renovation process of the meerschaum adsorbent that the present invention provides, by the adsorbent being adsorbed with debirs
It is passed through air, and is heated to 300-600 DEG C and carry out Regeneration Treatment, wherein semi-coke and adsorbed debirs burn completely again
Raw, and combustion process crosses liberated heat and can meet the required energy consumption of meerschaum regeneration, makes meerschaum obtain regeneration and activation.
Specific embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect become more apparent, below in conjunction with
The present invention will be described in further detail for embodiment.It should be appreciated that specific embodiment described herein is only in order to explain this
Invention, is not intended to limit the present invention.
Meerschaum is a kind of richness fibrous magnesium silicate clay mineral, and structure is in chain and Fiber Laminated shape, by 12 silicon
Oxygen tetrahedron and 8 magnesia its basic structural units of octahedra composition, meerschaum has big specific surface area, can adsorb a large amount of
Water and polar substancess.
Semi-coke, also known as semicoke, coke powder, is the solid product that low-disintegration coal is pyrolyzed gained at 400～600 DEG C, as one kind
New carbon material, it has, and fixed carbon is high, ratio resistance is high, chemism is high, containing the spy that ash is low, aluminum is low, sulfur is low, phosphorus is low
Property.
Describe preparation, the renovation process of meerschaum adsorbent below according to specific embodiment in detail.
Embodiment 1
The preparation method of meerschaum adsorbent:
Step s1, meerschaum pretreatment
It is washed to neutrality by after meerschaum acidification, and be dried to obtain pretreatment meerschaum；
Specifically, the hydrochloric acid using concentration as 0.2mol/l or nitric acid is as acid solution, by the meerschaum after pulverizing with described
Acid solution time of infusion, wherein meerschaum are 1:5 with the mass ratio of acid solution, then carry out filtering again, are washed with distillation
Wash to neutrality, under the conditions of 100 DEG C, 6h is dried, obtain pretreatment meerschaum；
Step s2, meerschaum are modified
Add organic solution to be impregnated in described pretreatment meerschaum, carry out after the completion of dipping filtering, wash, dry
Dry, grinding, then passes to nitrogen and is activated at 300-600 DEG C, obtain modified meerschaum；
Specifically, pretreatment meerschaum step s1 being obtained grinds after sieving the dodecyl for 1mmol/l in concentration
Impregnated in benzene sulfonic acid sodium salt solution, carry out after the completion of dipping filtering, the technique such as wash, dry, grinding, wherein drying temperature is
60-100 DEG C, grind size is 12-180 mesh, then passes to nitrogen, and high-temperature activation 2h under the conditions of 300 DEG C, obtains modified sea
Afrodite；
Step s3, adsorbent are prepared
The modified meerschaum that step s2 is obtained is mixed with semi-coke 1:10 in mass ratio, obtains meerschaum adsorbent, wherein
Semi-coke can be semi-coke raw material or modified semi-coke, and the granularity of semi-coke is 80-140 mesh, and the modified technique of modified semi-coke includes being acidified
Process and high-temperature activation, concrete technology refers to the modified technique of meerschaum.
It is organic that above-mentioned meerschaum adsorbent can be applicable to cationic dye wastewater, effluent containing heavy metal ions, toluene, formaldehyde etc.
Class waste water or a combination thereof.
Above-mentioned meerschaum adsorbent is applied to different types of waste water, effect is as follows:
Can be analyzed by above-mentioned data and draw, the adsorbable different types of waste water of meerschaum adsorbent of the present invention, by it
It is applied to cationic dye wastewater, heavy metal wastewater thereby, organic wastewater are adsorbed, wherein the absorption of cationic dye wastewater
Efficiency is 75-80%, and in heavy metal wastewater thereby, heavy metal adsorption efficiency is 80-83%, the absorption of toluene, formaldehyde in organic wastewater
Efficiency is 63-67%.
The adsorbent being adsorbed with waste is carried out Regeneration Treatment, obtains the meerschaum adsorbent regenerating, concrete technology is as follows:
It is passed through air in the adsorbent be adsorbed with waste, is heated to 300 DEG C, wherein semi-coke is complete with by adsorbed waste
Entirely burn and regenerate, and in combustion process, liberated heat is used for the activation of meerschaum, so that meerschaum is regenerated.
Embodiment 2
The preparation method of meerschaum adsorbent:
Step s1, meerschaum pretreatment
It is washed to neutrality by after meerschaum acidification, and be dried to obtain pretreatment meerschaum；
Specifically, the hydrochloric acid using concentration as 1.0mol/l or nitric acid is as acid solution, by the meerschaum after pulverizing with described
Acid solution time of infusion, wherein meerschaum are 1:20 with the mass ratio of acid solution, then carry out filtering again, are washed with distillation
Wash to neutrality, under the conditions of 105 DEG C, 5h is dried, obtain pretreatment meerschaum；
Step s2, meerschaum are modified
Add organic solution to be impregnated in described pretreatment meerschaum, carry out after the completion of dipping filtering, wash, dry
Dry, grinding, then passes to nitrogen and is activated under the conditions of 600 DEG C, obtain modified meerschaum；
Specifically, pretreatment meerschaum step s1 being obtained grinds after sieving the cetyl for 5mmol/l in concentration
Impregnated in trimethylammonium bromide solution, carry out after the completion of dipping filtering, the technique such as wash, dry, grinding, wherein dried temperature
Spend for 80 DEG C, grind size is 12-180 mesh, then passes to nitrogen, and high-temperature activation 2.5h under the conditions of 400 DEG C, obtains modification
Meerschaum；
Step s3, adsorbent are prepared
The modified meerschaum that step s2 is obtained is mixed with semi-coke 1:5 in mass ratio, obtains meerschaum adsorbent, wherein blue
Charcoal can be semi-coke raw material or modified semi-coke, and the granularity of semi-coke is 80-140 mesh, and the modified technique of modified semi-coke is included at acidifying
Reason and high-temperature activation, concrete technology refers to the modified technique of meerschaum.
It is organic that above-mentioned meerschaum adsorbent can be applicable to anionic dye waste water, effluent containing heavy metal ions, toluene, formaldehyde etc.
Class waste water or a combination thereof.
Above-mentioned meerschaum adsorbent is applied to different types of waste water, effect is as follows:
Can be analyzed by above-mentioned data and draw, the adsorbable different types of waste water of meerschaum adsorbent of the present invention, by it
It is applied to anionic dye waste water, heavy metal wastewater thereby, organic wastewater are adsorbed, wherein the absorption of cationic dye wastewater
Efficiency is 78-83%, and in heavy metal wastewater thereby, heavy metal adsorption efficiency is 77-80%, the absorption of toluene, formaldehyde in organic wastewater
Efficiency is 60-65%.
The adsorbent being adsorbed with waste is carried out Regeneration Treatment, obtains the meerschaum adsorbent regenerating, concrete technology is as follows:
It is passed through air in the adsorbent be adsorbed with waste, is heated to 400 DEG C, wherein semi-coke is complete with by adsorbed waste
Entirely burn and regenerate, and in combustion process, liberated heat is used for the activation of meerschaum, so that meerschaum is regenerated.
Embodiment 3
The preparation method of meerschaum adsorbent:
Step s1, meerschaum pretreatment
It is washed to neutrality by after meerschaum acidification, and be dried to obtain pretreatment meerschaum；
Specifically, the hydrochloric acid using concentration as 1.5mol/l or nitric acid is as acid solution, by the meerschaum after pulverizing with described
Acid solution time of infusion, wherein meerschaum are 1:10 with the mass ratio of acid solution, then carry out filtering again, are washed with distillation
Wash to neutrality, under the conditions of 120 DEG C, 4h is dried, obtain pretreatment meerschaum；
Step s2, meerschaum are modified
Add organic solution to be impregnated in described pretreatment meerschaum, carry out after the completion of dipping filtering, wash, dry
Dry, grinding, then passes to 600 DEG C of nitrogen and is activated, obtain modified meerschaum；
Specifically, pretreatment meerschaum step s1 being obtained grinds after sieving the dodecyl for 10mmol/l in concentration
Impregnated in benzene sulfonic acid sodium salt solution, carry out after the completion of dipping filtering, the technique such as wash, dry, grinding, wherein drying temperature is
100 DEG C, grind size is 12-180 mesh, then passes to nitrogen, and high-temperature activation 30min under the conditions of 600 DEG C, obtains modified sea
Afrodite；
Step s3, adsorbent are prepared
The modified meerschaum that step s2 is obtained is mixed with semi-coke 1:0.1 in mass ratio, obtains meerschaum adsorbent, wherein
Semi-coke can be semi-coke raw material or modified semi-coke, and the granularity of semi-coke is 80-140 mesh, and the modified technique of modified semi-coke includes being acidified
Process and high-temperature activation, concrete technology refers to the modified technique of meerschaum.
It is organic that above-mentioned meerschaum adsorbent can be applicable to cationic dye wastewater, effluent containing heavy metal ions, toluene, formaldehyde etc.
Class waste water or a combination thereof.
Above-mentioned meerschaum adsorbent is applied to different types of waste water, effect is as follows:
Can be analyzed by above-mentioned data and draw, the adsorbable different types of waste water of meerschaum adsorbent of the present invention, by it
It is applied to cationic dye wastewater, heavy metal wastewater thereby, organic wastewater are adsorbed, wherein the absorption of cationic dye wastewater
Efficiency is 70-75%, and in heavy metal wastewater thereby, heavy metal adsorption efficiency is 73%, the absorption effect of toluene, formaldehyde in organic wastewater
Rate is 57-60%.
The adsorbent being adsorbed with waste is carried out Regeneration Treatment, obtains the meerschaum adsorbent regenerating, concrete technology is as follows:
It is passed through air in the adsorbent be adsorbed with waste, is heated to 600 DEG C, wherein semi-coke is complete with by adsorbed waste
Entirely burn and regenerate, and in combustion process, liberated heat is used for the activation of meerschaum, so that meerschaum is regenerated.
Meerschaum adsorbent providing compared to prior art, the present invention and preparation method thereof, renovation process beneficial effect
It is:
First, the preparation method of the meerschaum adsorbent that the present invention provides, with the meerschaum of loose structure and semi-coke as raw material,
The meerschaum adsorbent absorption property obtaining is excellent；By adjusting the ratio of meerschaum and semi-coke, can be applicable to different types of useless
Water process, thus improve its range of application；
2nd, the meerschaum adsorbent that the present invention provides, with the meerschaum of loose structure and semi-coke as raw material, with low cost.
3rd, the renovation process of the meerschaum adsorbent that the present invention provides, by the adsorbent being adsorbed with debirs
It is passed through air, and is heated to 300-600 DEG C and carry out Regeneration Treatment, wherein semi-coke and adsorbed debirs burn completely again
Raw, and combustion process crosses liberated heat and can meet the required energy consumption of meerschaum regeneration, makes meerschaum obtain regeneration and activation.
The foregoing is only embodiments of the invention, not thereby limit the present invention the scope of the claims, every using this
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in the technology neck of other correlations
Domain, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of meerschaum adsorbent is it is characterised in that comprise the steps:
Meerschaum pretreatment: be washed to neutrality by after meerschaum acidification, and be dried to obtain pretreatment meerschaum；
Meerschaum is modified: adds organic solution to be impregnated in described pretreatment meerschaum, carries out filtering, water after the completion of dipping
Wash, dry, grind, then pass to nitrogen and activated under the conditions of 300-600 DEG C, obtain modified meerschaum；
Adsorbent is prepared: modified meerschaum is mixed in proportion with semi-coke, obtains meerschaum adsorbent.
2. the preparation method of meerschaum adsorbent according to claim 1 is it is characterised in that described meerschaum modification procedure
In, organic solution is dodecylbenzene sodium sulfonate or cetyl trimethylammonium bromide, and the concentration of described organic solution is 1-
10mmol/l.
3. the preparation method of meerschaum adsorbent according to claim 2 is it is characterised in that described meerschaum modification procedure
In, soak time is 30-180min.
4. the preparation method of meerschaum adsorbent according to claim 1 is it is characterised in that described meerschaum pretreatment walks
In rapid, the acid solution used by meerschaum acidification technique is nitric acid or hydrochloric acid, and solubility is 0.2-1.5mol/l.
5. the preparation method of meerschaum adsorbent according to claim 4 is it is characterised in that the matter of meerschaum and acid solution
Amount ratio is 1:5-20.
6. the preparation method of meerschaum adsorbent according to claim 5 is it is characterised in that described meerschaum pretreatment walks
In rapid, baking temperature is 100-120 DEG C.
7. the preparation method of meerschaum adsorbent according to claim 1 is it is characterised in that described adsorbent preparation steps
In, modified meerschaum is 1:0.1-10 with the mass ratio of semi-coke.
8. the preparation method of meerschaum adsorbent according to claim 7 is it is characterised in that described adsorbent preparation steps
In, the granularity of described modified meerschaum is 12-180 mesh, and the granularity of described semi-coke is 80-140 mesh.
9. a kind of meerschaum adsorbent is it is characterised in that by the meerschaum adsorbent any one of claim 1 to 8
Preparation method prepares.
10. a kind of renovation process of the meerschaum adsorbent described in claim 9 is it is characterised in that include: by described meerschaum
After adsorbent is used for adsorbing waste water, in the adsorbent be adsorbed with waste, it is passed through air, and is heated to 300-600 DEG C and regenerated
Process, obtain the meerschaum adsorbent regenerating.
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| CN112044403A (en) * | 2020-09-07 | 2020-12-08 | 湘潭大学 | Preparation method and application of sepiolite-based formaldehyde adsorbent |
| CN113023820A (en) * | 2021-03-25 | 2021-06-25 | 韩玉 | Low-cost and efficient municipal sewage treatment method |
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| CN107262044A (en) * | 2017-07-01 | 2017-10-20 | 湘潭大学 | It is a kind of to Congo red magnetic coupling functional material with efficient clearance and preparation method thereof in water |
| CN108083944A (en) * | 2017-12-22 | 2018-05-29 | 西安建筑科技大学 | A kind of soil conditioner and preparation method thereof |
| CN108325504B (en) * | 2018-02-28 | 2019-10-11 | 武汉大学 | A kind of method of natural layered silicate nanoparticle and the charcoal secondary absorption removal dye of positive ion |
| CN108325504A (en) * | 2018-02-28 | 2018-07-27 | 武汉大学 | A kind of method of natural layered silicate nanoparticle and the charcoal secondary absorption removal dye of positive ion |
| CN108654578A (en) * | 2018-04-17 | 2018-10-16 | 湖南大学 | A kind of meerschaum adsorbent and its preparation method and application that amino silane grafting is modified |
| CN111298761A (en) * | 2018-12-12 | 2020-06-19 | 西北大学 | Modified sepiolite adsorbent and preparation method and application thereof |
| CN111298761B (en) * | 2018-12-12 | 2023-04-07 | 西北大学 | Modified sepiolite adsorbent and preparation method and application thereof |
| CN109865503A (en) * | 2019-03-20 | 2019-06-11 | 安徽工业大学 | A kind of magnetic conductive polymer/sepiolite/humic acid complex microsphere preparation and its application |
| CN112044403A (en) * | 2020-09-07 | 2020-12-08 | 湘潭大学 | Preparation method and application of sepiolite-based formaldehyde adsorbent |
| CN113023820A (en) * | 2021-03-25 | 2021-06-25 | 韩玉 | Low-cost and efficient municipal sewage treatment method |
| CN113023820B (en) * | 2021-03-25 | 2024-06-21 | 北京双傲生态环境技术有限公司 | Low-cost and high-efficiency urban sewage treatment method |
| CN115849492A (en) * | 2022-11-22 | 2023-03-28 | 核工业北京化工冶金研究院 | Method for treating uranium-containing acidic wastewater |
| CN116730466A (en) * | 2023-06-16 | 2023-09-12 | 上海永丰热镀锌有限公司 | Iron removal purification treatment process for hot galvanizing acid rinsing wastewater |
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