CN106732434A - A kind of method that acticarbon is prepared based on humic acid dipping - Google Patents
A kind of method that acticarbon is prepared based on humic acid dipping Download PDFInfo
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- CN106732434A CN106732434A CN201710062893.6A CN201710062893A CN106732434A CN 106732434 A CN106732434 A CN 106732434A CN 201710062893 A CN201710062893 A CN 201710062893A CN 106732434 A CN106732434 A CN 106732434A
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- Prior art keywords
- activated carbon
- humic acid
- acticarbon
- prepared based
- dipping
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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
- B01J20/28054—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 surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
-
- 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
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3214—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
-
- 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
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
Abstract
The invention discloses a kind of method that acticarbon is prepared based on humic acid dipping, by with activated carbon as raw material, add it to carry out impregnating modified in treated humic acid solution, the enhanced acticarbon of heavy metal adsorption capacity is obtained by the way that dipping is modified, because humic acid is generally the accessory substance of generation during waste treatment process, the present invention processes activated carbon as maceration extract in deionized water by the use of humic acid dissolving, realize waste carries out recycling again, in the case where ensureing that obtained acticarbon has superperformance, promote economic circulation.
Description
Technical field
It is especially a kind of that acticarbon is prepared based on humic acid dipping the present invention relates to acticarbon field
Method.
Background technology
With expanding economy and the progressively quickening of process of industrialization, its environmental problem brought therewith is increasingly subject to people
Concern.According to statistics, the industrial wastewater about 8 × 10 of China's discharge every year8m3, wherein containing heavy metal in chromium, zinc, nickel, lead, mercury
The waste water of ion is once discharged into river or underground water, it will the harm for being difficult to retrieve is caused, due to these heavy metal ion
With stability and extremely strong toxicity higher, these waste water are processed using traditional water treatment technology, not only consume a large amount of
The energy, it is also possible to produce secondary waste, because activated carbon has huge specific surface area, abundant pore structure, thing higher
Reason absorption and chemisorbed, with preferable water treatment effect, therefore are widely used in the treatment of waste water.
Because normal activated carbon specific surface area is about in 500~1500m2/ g, its Selective adsorption is relatively poor, specific surface
The low, adsorption capacity of product is limited, and the particular/special requirement of current heavy metal pollution treatment can not have been met, and this is caused to high-specific surface area
The demand of activated carbon constantly rises.
Heavy metal ion absorption on the activated carbon is not only simple physical absorption, usually with the surface official of activated carbon
Can roll into a ball carries out reaction formation precipitation and complex compound or carries out ion exchange etc., due to the special nature of heavy metal ion so that
, it is necessary to be improved in preparation technology when preparing activated carbon, optimize the surface functional group of activated carbon, lift the absorption of activated carbon
Ability.
Conventional chemical methods prepare the property charcoal of Adsorption of Heavy Metals, and mainly to use highly basic KOH, NaOH etc. be activator, due to nothing
The poor compatibility of machine alkali and carbon structure, although the activated carbon specific surface area that result in preparation is big, in the pore structure of activated carbon
Functional group is few, and the adsorption capacity of heavy metal is poor, therefore, be improve active carbon pore structure on functional group number, using with carbon knot
It is a kind of brand-new Research Thinking that the good organic base of structure compatibility activate.
The content of the invention
In order to solve the deficiencies in the prior art, the present invention provides a kind of easy to operate, implementation reliability, can strengthen activated carbon
The method that acticarbon is prepared based on humic acid dipping of heavy metal adsorption capacity.
In order to realize above-mentioned technical purpose, the technical scheme is that：
A kind of method that acticarbon is prepared based on humic acid dipping, with activated carbon as raw material, is added into everywhere
Dipping is carried out in the humic acid solution managed modified, inhaled by the modified enhanced activated carbon of heavy metal adsorption capacity that is obtained of dipping
Attached dose.
Further, the method that acticarbon is prepared based on humic acid dipping, it is comprised the following steps：
(1) Activated Carbon Pretreatment：Activated carbon is washed and prepared Powdered Activated Carbon is dried, then obtained powder is lived
Property charcoal is deposited in drying box；
(2) solid humic acid is added in deionized water, and adjusts solution ph after 7~9, to be stirred dissolving 18
~24h, is obtained suspension；
(3) toward inorganic flocculating agent is added in suspension obtained above, through mixing, standing, after centrifugation, then by humic acid
Clear liquid is pipetted out；
(4) Powdered Activated Carbon obtained in step (1) is impregnated into the humic acid supernatant of step (3) separation, and is adjusted
Maceration extract pH value to neutrality, then will add Powdered Activated Carbon maceration extract be placed in constant temperature oscillator carry out vibration 40~
48h, after vibration terminates, the Powdered Activated Carbon in maceration extract is leached, and is vacuum dried again after being washed with distilled water,
Can be prepared by acticarbon.
Further, after activated carbon is washed with distilled water in the step (1), it is placed on temperature and is set as 100
DEG C baking oven in dry 4h, be obtained Powdered Activated Carbon.
Further, the rotten plant in deionized water is added in the activated carbon and step (2) that are impregnated in the step (4)
Sour mass ratio is 1: 0.25~1.5.
Further, the inorganic flocculating agent in the step (3) be ferric sulfate, aluminum sulfate, aluminium chloride, ferrous sulfate in extremely
A kind of few mixing composition.
Further, add in the step (3) flocculant to be mixed, stand after suspension in 5000~8000r/
After carrying out 10~15min of centrifugation under the rotating speed of min, then pipette humic acid supernatant.
Further, the maceration extract for Powdered Activated Carbon being added in the step (4) is set as 23~27 DEG C, speed in temperature
To carry out 42~48h of vibration in the constant temperature oscillator of 120~180r/min.
Further, the Powdered Activated Carbon for being leached in the step (4) enters after distilling water washing under conditions of 110 DEG C
Row vacuum drying 6h.
Preferably, above-mentioned activated carbon is commercial activated carbons.
Using above-mentioned technical scheme, beneficial effects of the present invention are：Maceration extract is prepared using humic acid, by by advance
Activated carbon after treatment is immersed in the humic acid supernatant pipetted after flocculation and centrifugation, and activated carbon is carried out by infusion process
It is modified, the adsorption capacity of activated carbon heavy metal ion is remarkably reinforced, improve the adsorption capacity of activated carbon.
Specific embodiment
A kind of method that acticarbon is prepared based on humic acid dipping, with activated carbon as raw material, is added into everywhere
Dipping is carried out in the humic acid solution managed modified, inhaled by the modified enhanced activated carbon of heavy metal adsorption capacity that is obtained of dipping
Attached dose.
Further, the method that acticarbon is prepared based on humic acid dipping, it is comprised the following steps：
(1) Activated Carbon Pretreatment：Activated carbon is washed and prepared Powdered Activated Carbon is dried, then obtained powder is lived
Property charcoal is deposited in drying box；
(2) solid humic acid is added in deionized water, and adjusts solution ph after 7~9, to be stirred dissolving 18
~24h, is obtained suspension；
(3) toward inorganic flocculating agent is added in suspension obtained above, through mixing, standing, after centrifugation, then by humic acid
Clear liquid is pipetted out；
(4) Powdered Activated Carbon obtained in step (1) is impregnated into the humic acid supernatant of step (3) separation, and is adjusted
Maceration extract pH value to neutrality, then will add Powdered Activated Carbon maceration extract be placed in constant temperature oscillator carry out vibration 40~
48h, after vibration terminates, the Powdered Activated Carbon in maceration extract is leached, and is vacuum dried again after being washed with distilled water,
Can be prepared by acticarbon.
Further, after activated carbon is washed with distilled water in the step (1), it is placed on temperature and is set as 100
DEG C baking oven in dry 4h, be obtained Powdered Activated Carbon.
Further, the rotten plant in deionized water is added in the activated carbon and step (2) that are impregnated in the step (4)
Sour mass ratio is 1: 0.25~1.5.
Further, the inorganic flocculating agent in the step (3) be ferric sulfate, aluminum sulfate, aluminium chloride, ferrous sulfate in extremely
A kind of few mixing composition.
Further, add in the step (3) flocculant to be mixed, stand after suspension in 5000~8000r/
After carrying out 10~15min of centrifugation under the rotating speed of min, then pipette humic acid supernatant.
Further, the maceration extract for Powdered Activated Carbon being added in the step (4) is set as 23~27 DEG C, speed in temperature
To carry out 42~48h of vibration in the constant temperature oscillator of 120~180r/min.
Further, the Powdered Activated Carbon for being leached in the step (4) enters after distilling water washing under conditions of 110 DEG C
Row vacuum drying 6h.
Preferably, above-mentioned activated carbon is commercial activated carbons.
Embodiment 1
The method that acticarbon is prepared based on humic acid dipping, it is comprised the following steps：
(1) Activated Carbon Pretreatment：Take commercial activated carbons and wash and be placed in drying 4h in 100 DEG C of baking oven, powder is obtained
Last activated carbon, then obtained Powdered Activated Carbon deposited in into drying box；
(2) 0.25g solid humic acids are added in 100ml deionized waters, and adjust solution ph after 7, to be stirred
Dissolving 24h is mixed, suspension is obtained；
(3) toward ferric sulfate is added in suspension obtained above, after mixing, standing, it is transferred in centrifuge with 6000r/
After the speed of min carries out centrifugation 12min, then humic acid supernatant is pipetted out；
(4) Powdered Activated Carbon obtained in taking 1g steps (1) is impregnated into the humic acid supernatant of step (3) separation, and is adjusted
To neutrality, the maceration extract that then will add Powdered Activated Carbon is placed in constant temperature oscillator with 23 DEG C of temperature section maceration extract pH value
The rotating speed of condition and 180r/min carries out vibration 42h, after vibration terminates, the Powdered Activated Carbon in maceration extract is leached, and
After being washed with distilled water, vacuum drying 6h is carried out under the conditions of 110 DEG C, you can acticarbon is obtained.
Embodiment 2
The method that acticarbon is prepared based on humic acid dipping, it is comprised the following steps：
(1) Activated Carbon Pretreatment：Take commercial activated carbons and wash and be placed in drying 4h in 100 DEG C of baking oven, powder is obtained
Last activated carbon, then obtained Powdered Activated Carbon deposited in into drying box；
(2) 0.5g solid humic acids are added in 100ml deionized waters, and adjust solution ph after 8, to be stirred
Dissolving 20h, is obtained suspension；
(3) toward aluminum sulfate is added in suspension obtained above, after mixing, standing, it is transferred in centrifuge with 5000r/
After the speed of min carries out centrifugation 15min, then humic acid supernatant is pipetted out；
(4) Powdered Activated Carbon obtained in taking 1g steps (1) is impregnated into the humic acid supernatant of step (3) separation, and is adjusted
To neutrality, the maceration extract that then will add Powdered Activated Carbon is placed in constant temperature oscillator with 25 DEG C of temperature section maceration extract pH value
The rotating speed of condition and 120r/min carries out vibration 48h, after vibration terminates, the Powdered Activated Carbon in maceration extract is leached, and
After being washed with distilled water, vacuum drying 6h is carried out under the conditions of 110 DEG C, you can acticarbon is obtained.
Embodiment 3
The method that acticarbon is prepared based on humic acid dipping, it is comprised the following steps：
(1) Activated Carbon Pretreatment：Take commercial activated carbons and wash and be placed in drying 4h in 100 DEG C of baking oven, powder is obtained
Last activated carbon, then obtained Powdered Activated Carbon deposited in into drying box；
(2) 1g solid humic acids are added in 100ml deionized waters, and adjust solution ph after 9, to be stirred molten
Solution 18h, is obtained suspension；
(3) toward aluminium chloride is added in suspension obtained above, after mixing, standing, it is transferred in centrifuge with 8000r/
After the speed of min carries out centrifugation 10min, then humic acid supernatant is pipetted out；
(4) Powdered Activated Carbon obtained in taking 1g steps (1) is impregnated into the humic acid supernatant of step (3) separation, and is adjusted
To neutrality, the maceration extract that then will add Powdered Activated Carbon is placed in constant temperature oscillator with 27 DEG C of temperature section maceration extract pH value
The rotating speed of condition and 150r/min carries out vibration 45h, after vibration terminates, the Powdered Activated Carbon in maceration extract is leached, and
After being washed with distilled water, vacuum drying 6h is carried out under the conditions of 110 DEG C, you can acticarbon is obtained.
Embodiment 4
The method that acticarbon is prepared based on humic acid dipping, it is comprised the following steps：
(1) Activated Carbon Pretreatment：Take commercial activated carbons and wash and be placed in drying 4h in 100 DEG C of baking oven, powder is obtained
Last activated carbon, then obtained Powdered Activated Carbon deposited in into drying box；
(2) 1.5g solid humic acids are added in 100ml deionized waters, and adjust solution ph after 8, to be stirred
Dissolving 18h, is obtained suspension；
(3) toward the mixture of addition ferric sulfate and ferrous sulfate in suspension obtained above, after mixing, standing, turn
Entering after carry out centrifugation 15min with the speed of 6000r/min in centrifuge, then humic acid supernatant being pipetted out；
(4) Powdered Activated Carbon obtained in taking 1g steps (1) is impregnated into the humic acid supernatant of step (3) separation, and is adjusted
To neutrality, the maceration extract that then will add Powdered Activated Carbon is placed in constant temperature oscillator with 25 DEG C of temperature section maceration extract pH value
The rotating speed of condition and 150r/min carries out vibration 45h, after vibration terminates, the Powdered Activated Carbon in maceration extract is leached, and
After being washed with distilled water, vacuum drying 6h is carried out under the conditions of 110 DEG C, you can acticarbon is obtained.
Cu2+Adsorption experiment is tested
Acticarbon obtained in 20mg above-described embodiments 1~4 is taken respectively to be separately added into after carrying out detection specific surface area
To equipped with the Cu that 40ml concentration is 6.18mg/L2+Carry out being divided into 4 groups in the centrifuge tube of solution, then take 20mg commercial powder activated carbons
Be added to equipped with the Cu that 40ml concentration is 6.18mg/L after detecting specific surface area detection2+As control in the centrifuge tube of solution
Group, is respectively adjusted to 4 the pH of each group sample solution, and Cu is detected after carrying out vibration 2h with the speed of 120r/min at room temperature2+
Absorptivity, obtain result as follows：
The above is embodiments of the invention, for the ordinary skill in the art, religion of the invention
Lead, without departing from the principles and spirit of the present invention all impartial changes done according to scope of the present invention patent, repair
Change, replace and modification, should all belong to covering scope of the invention.
Claims (9)
1. a kind of method that acticarbon is prepared based on humic acid dipping, it is characterised in that：With activated carbon as raw material, by it
It is added in treated humic acid solution that to carry out dipping modified, it is enhanced by the modified prepared heavy metal adsorption capacity of dipping
Acticarbon.
2. the method that acticarbon is prepared based on humic acid dipping according to claim 1, it is characterised in that：Its bag
Include following steps：
（1）Activated Carbon Pretreatment：Activated carbon is washed and prepared Powdered Activated Carbon is dried, then by obtained Powdered Activated Carbon
In depositing in drying box；
（2）Solid humic acid is added in deionized water, and adjust solution ph for after 7~9, be stirred dissolving 18~
24h, is obtained suspension；
（3）Inorganic flocculating agent is added toward suspension obtained above, through mixing, standing, after centrifugation, then by humic acid supernatant
Pipette out；
（4）By step（1）Obtained Powdered Activated Carbon is impregnated into step（3）In the humic acid supernatant of separation, and adjust dipping
To neutrality, the maceration extract that then will add Powdered Activated Carbon is placed in 40~48h of vibration is carried out in constant temperature oscillator liquid pH value, shakes
After swinging end, the Powdered Activated Carbon in maceration extract is leached, and be vacuum dried again after being washed with distilled water, you can system
Obtain acticarbon.
3. the method that acticarbon is prepared based on humic acid dipping according to claim 2, it is characterised in that：It is described
Step（1）It is middle activated carbon is washed with distilled water after, be placed on temperature and be set as drying 4h in 100 DEG C of baking oven, make
Obtain Powdered Activated Carbon.
4. the method that acticarbon is prepared based on humic acid dipping according to claim 2, it is characterised in that：It is described
Step（4）In the activated carbon that is impregnated and step（2）In to be added to humic acid mass ratio in deionized water be 1：0.25~
1.5。
5. the method that acticarbon is prepared based on humic acid dipping according to claim 2, it is characterised in that：It is described
Step（3）In inorganic flocculating agent be at least one mixing composition in ferric sulfate, aluminum sulfate, aluminium chloride, sulfuric acid smelting iron.
6. the method that acticarbon is prepared based on humic acid dipping according to claim 2, it is characterised in that：It is described
Step（3）It is middle add flocculant mixed, stand after suspension centrifugation 10 is carried out under the rotating speed of 5000~8000r/min
After~15min, then pipette humic acid supernatant.
7. the method that acticarbon is prepared based on humic acid dipping according to claim 2, it is characterised in that：It is described
Step（4）In add the maceration extract of Powdered Activated Carbon and be set as 23~27 DEG C in temperature, speed is the perseverance of 120~180r/min
42~48h of vibration is carried out in warm oscillator.
8. the method that acticarbon is prepared based on humic acid dipping according to claim 2, it is characterised in that：It is described
Step（4）In the Powdered Activated Carbon that leaches after distilling water washing, vacuum drying 6h is carried out under conditions of 110 DEG C.
9. the method that acticarbon is prepared based on humic acid dipping according to any of the above-described claim, its feature is existed
In：Described activated carbon is commercial activated carbons.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993448A (en) * | 2018-09-10 | 2018-12-14 | 芜湖新达园林绿化集团有限公司 | A kind of Low Cost Sorbents and its preparation method and application |
| CN108993435A (en) * | 2018-09-10 | 2018-12-14 | 黑龙江明强科技有限公司 | Superpower absorbent-type polyaluminium aluminium base flocculant |
| CN109012632A (en) * | 2018-09-10 | 2018-12-18 | 芜湖新达园林绿化集团有限公司 | The preparation and application of a kind of adhesive flocculant complex microsphere and adhesive flocculant |
| CN109550483A (en) * | 2018-12-07 | 2019-04-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Compound adsorbent and preparation method thereof and application method |
| CN111921501A (en) * | 2020-05-09 | 2020-11-13 | 四川师范大学 | Iron-carrying humic acid and preparation method, application and application method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993448A (en) * | 2018-09-10 | 2018-12-14 | 芜湖新达园林绿化集团有限公司 | A kind of Low Cost Sorbents and its preparation method and application |
| CN108993435A (en) * | 2018-09-10 | 2018-12-14 | 黑龙江明强科技有限公司 | Superpower absorbent-type polyaluminium aluminium base flocculant |
| CN109012632A (en) * | 2018-09-10 | 2018-12-18 | 芜湖新达园林绿化集团有限公司 | The preparation and application of a kind of adhesive flocculant complex microsphere and adhesive flocculant |
| CN109550483A (en) * | 2018-12-07 | 2019-04-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Compound adsorbent and preparation method thereof and application method |
| CN111921501A (en) * | 2020-05-09 | 2020-11-13 | 四川师范大学 | Iron-carrying humic acid and preparation method, application and application method thereof |
| CN111921501B (en) * | 2020-05-09 | 2023-04-11 | 四川师范大学 | Iron-carrying humic acid and preparation method, application and application method thereof |
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