CN108786723A - Utilize the method for estrogen in activation montmorillonite biology carbon composite removal water body - Google Patents
Utilize the method for estrogen in activation montmorillonite biology carbon composite removal water body Download PDFInfo
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- CN108786723A CN108786723A CN201710303997.1A CN201710303997A CN108786723A CN 108786723 A CN108786723 A CN 108786723A CN 201710303997 A CN201710303997 A CN 201710303997A CN 108786723 A CN108786723 A CN 108786723A
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- montmorillonite
- estrogen
- carbon composite
- activation
- biology carbon
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
Abstract
The application that the present invention relates to montmorillonite composite materials in water treatment field, discloses a kind of method removing estrogen in water using activation montmorillonite biology carbon composite, and method summarizes following steps, composite material preparation：Montmorillonite and husk biomass are mixed, carry out hydrothermal carbonization, then activated with KOH to gained montmorillonite biology carbon composite；Minimizing technology includes the following steps：Activation montmorillonite biology carbon composite is added in estrogen solution, is vibrated, completes the Adsorption to estrogen.The present invention efficiently eliminates estrogen in water, reduces harm of the estrogen to aquatic ecological environment, while activating montmorillonite biology carbon composite to realize the purpose of cycling and reutilization by using activation montmorillonite biology charcoal composite material adsorbent.
Description
Technical field
The application that the present invention relates to montmorillonite composite materials in water treatment field is related to a kind of utilize and activates montmorillonite life
Object carbon composite removes the application of estrogen in water body.
Background technology
Incretion interferent is universally present in water body, even in drinking water.Incretion interferent can interfere people and
Wildlife species maintain the regulation and control of homeostasis and evolution.Meanwhile estrogen is considered to have extremely strong endocrine disruption
Property and bioactivity, human body or animals' reproduction obstacle, abnormal behavior and young variation can be caused at much lower concentrations.Both at home and abroad
The testing result of many water bodys shows to be prevalent in using estradiol and ethinyloestradiol as the estrogen of representative in urban water-body and dense
It spends and is higher than interference threshold more, and incomplete removal of these major parts because of sewage treatment plant to this substance.This results in river
In flowing water body there are potential risks in fish and other aquatiles at low concentrations.Currently used minimizing technology mainly has biology
Facture, advanced oxidation processes and absorption method.Absorption method is substantially attraction of the adsorbent activity surface to estrogen, and Yin Qigao
Effect, the advantages that low price and recuperability are strong, receive more and more attention, and commonly use the active charcoal of adsorbent, multi-walled carbon nanotube
Deng.
In recent years, the application of montmorillonite material receives significant attention.Since the height absorption to Cationic chemistry is affine
Power and its unique performance, such as big surface area, unique layer structure, low cost and highly expanded, montmorillonite are used in doctor
It treats and environmental pollution treatment field.Domestic and international many scholars handle the organic pollution in water body and soil to montmorillonite and carry out
Correlative study.Meanwhile charcoal organic material is due to structures such as loose porous, aligned orderly aromatic rings lamellas so that
Charcoal has prodigious potentiality in terms of the pollutants such as heavy metal, organic matter, dyestuff in adsorbing waste water.Furthermore composite material
Use scope be also concerned, they have the function of the features such as removal efficiency is high, operating cost is low, modification is easy.Therefore, it examines
More than worry, montmorillonite and husk biomass are mixed, hydrothermal carbonization, then material is activated, montmorillonite table is increased with this
The estrogen adsorption site in face and the value volume and range of product of functional group, to improve its adsorption capacity to estrogen.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a kind of at low cost, adsorption efficiency
High, recycling property activates by force and to strong the utilizing of contaminant removal capacity female in montmorillonite biology carbon composite removal water body
The method of hormone.
In order to solve the above technical problems, technical solution proposed by the present invention is multiple using the montmorillonite charcoal of hydrothermal carbonization
The method that estrogen in water body is removed after condensation material is activated, includes the following steps：By montmorillonite and husk biomass mixing water
Heat carbonization, then carries out KOH activation to it；The obtained composite material completes the Adsorption to estrogen.
In the above-mentioned method using estrogen in activation montmorillonite biology carbon composite removal water, the activation is covered de-
Stone biology carbon composite is through the following steps that be prepared：
(1) montmorillonite and charcoal are mixed, are dissolved in 70mL ultra-pure waters, this suspension is placed in 100mL reaction kettles,
It in being heated in drying box, cools down, then it is thoroughly washed repeatedly with deionized water, methanol washing by soaking filters, drying.
(2) KOH is added in montmorillonite biology carbon composite after drying in step (1) to activate, is activated
Montmorillonite biology carbon composite afterwards.
In the above-mentioned method using estrogen in activation montmorillonite biology carbon composite removal water, the activation is covered de-
In the preparation process (1) of stone biology carbon composite, the montmorillonite and charcoal mixed proportion are 1:1, in the drying box
Heating condition：Temperature is 180 DEG C, time 16h.
In the above-mentioned method using estrogen in activation montmorillonite biology carbon composite removal water, the activation is covered de-
In the preparation process (2) of stone biology carbon composite, the ratio that KOH and montmorillonite biology carbon composite is added is 1%, activation
Time is 4h.
In the above-mentioned method using estrogen in activation montmorillonite biology carbon composite removal water, in the water body
Estrogen is two kinds, estradiol and female alkynol.
In the above-mentioned method using estrogen in activation montmorillonite biology carbon composite removal water, in the water body
The control of the concentration of estradiol and female alkynol is controlled in 0.2-8.0mg/L, pH in 3.0-11.0, and temperature control is in 25 DEG C, rotating speed
170rpm。
In the above-mentioned method using estrogen in activation montmorillonite biology carbon composite removal water, in the water body
The equilibrium adsorption capacity of estradiol and female alkynol respectively reaches 114 and 69mg/g.
Compared with the prior art, the advantages of the present invention are as follows：
1. the present invention provides a kind of method of estrogen in montmorillonite biology carbon composite removal water using activation, lead to
It crosses and montmorillonite is handled using hydrothermal carbonization, change montmorillonite surface characteristics, realize and estrogen is effectively removed；
2. the activation montmorillonite biology carbon composite of the present invention has, easy to operate, operating cost is low, surface functionalities
Group is more and the characteristics of easily combination with estrogen molecule, and removal efficiency is high, has environment friendly, for estrogen in water body
Removal proposes new method；
3. the raw material sources of the present invention are abundant, at low cost, and preparation method and simple for process, it can effectively realize work
Industry metaplasia is produced.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of pristine montmorillonite
Fig. 2 is the scanning electron microscope (SEM) photograph that montmorillonite biology carbon composite is activated in present example 1
Fig. 3 is suction of the activation montmorillonite biology carbon composite to estrogen under the differential responses time in present example 2
Attached variation
Fig. 4 is suction of the activation montmorillonite biology carbon composite to estrogen under different initial concentrations in present example 3
Attached variation
Fig. 5 is absorption of the activation montmorillonite biology carbon composite to estrogen under condition of different pH in present example 4
Variation
Fig. 6 is the absorption variation that circular regeneration activates montmorillonite biology carbon composite to estrogen in present example 5
Specific implementation mode
The present invention is described in further details below with reference to Figure of description and specific embodiment.
Embodiment 1
A kind of method that present invention activation montmorillonite biology carbon composite removes estrogen in water body, including following step
Suddenly：
(1) activation montmorillonite biology carbon composite is prepared
(1.1) by montmorillonite (Fig. 1) and charcoal with 1:1 ratio mixing, is dissolved in 70mL ultra-pure waters, by this suspension
It is placed in 100mL reaction kettles, in heating 16h in 180 DEG C of drying boxes, cools down.
(1.2) montmorillonite and charcoal mixed liquor that step (1.1) obtains thoroughly are washed three times with deionized water, methanol
Washing by soaking three times, in 80 DEG C of drying boxes dry for 24 hours by filtering.
(1.3) KOH is added in the montmorillonite biology carbon composite in step (1.2) after drying, KOH gives birth to montmorillonite
The mass fraction ratio of object carbon composite is 1%, is activated, soak time 4h, last 80 DEG C of drying, and grinding is lived
Montmorillonite biology carbon composite after change, as shown in Figure 2.Fig. 2 is the activation montmorillonite charcoal composite wood in the present embodiment
The electron scanning electron microscope of material.Comparison diagram 1 and Fig. 2 are it is found that the activation montmorillonite charcoal composite material surface of the present invention has one
Layer charcoal package, rough surface, aggregation extent are high.
(2) in water body estrogen Adsorption
(2.1) storing solution of 2.5mg/mL estradiol and ethinyloestradiol is prepared：It weighs estradiol or ethinyloestradiol 0.125g is dissolved in
In 50mL deionized waters, it is stored in 4 DEG C of refrigerators.
(2.2) storing solution in (2.1) is diluted to aimed concn, activation montmorillonite prepared by 5mg steps (1.3) is added
Biological carbon composite is placed in 25 DEG C of constant temperature oscillations, and water-bath constant temperature oscillator rotating speed is 170rpm, and duration of oscillation is for 24 hours, instead
Ying Hou, solution sedimentation, using 0.45 μm of Teflon filtration (syringe type).
(2.3) the solution concentration Ultraluminescence photometric determination after being reacted (2.2).
Embodiment 2
A kind of method that the activation montmorillonite biology carbon composite of the present invention removes estrogen in water body, step and reality
The Adsorption for applying estrogen in 1 water body of example is identical, is different only in that：Sorption reaction time is 0-24h in embodiment 2.
The activation montmorillonite life obtained of 5mg embodiments 1 is added in the estrogen solution of a concentration of 6mg/L after taking 100mL to dilute
Object carbon composite is placed in 25 DEG C of constant temperature oscillations, water-bath constant temperature oscillator rotating speed be 170rpm, duration of oscillation 0-24h, instead
Ying Hou, solution sedimentation, using 0.45 μm of Teflon filtration (syringe type).It is molten after being reacted with Ultraluminescence photometric determination
The adsorbance result of the concentration of estrogen in liquid, calculating is shown in Fig. 3.The result shows that activation montmorillonite biology carbon composite is to female two
The adsorbance of alcohol and ethinyloestradiol is higher than pristine montmorillonite, and the incipient rate of adsorption is most fast, with the incremental rate of adsorption of time
It gradually tends towards stability, respectively in 6h and 4h close to adsorption equilibrium.Meanwhile montmorillonite biology carbon composite is activated to estradiol
Adsorption effect is higher than ethinyloestradiol.
Embodiment 3
A kind of method that the activation montmorillonite biology carbon composite of the present invention removes estrogen in water body, step and reality
The Adsorption for applying estrogen in 1 water body of example is identical, is different only in that：It is 0.2-8.0mg/ that initial concentration is adsorbed in embodiment 3
L。
A concentration of 0.2 after taking 100mL to dilute, 0.4,0.6,0.8,1.0,2.0,3.0,4.0,5.0,6.0,7.0 He
The estrogen solution of 8.0mg/L is added the activation montmorillonite biology carbon composite obtained of 5mg embodiments 1, is placed in 25 DEG C of constant temperature
In oscillation, water-bath constant temperature oscillator rotating speed is 170rpm, and duration of oscillation is that for 24 hours, after reaction, solution sedimentation is poly- using 0.45 μm
Tetrafluoroethene filters (syringe type).With the concentration of estrogen in solution after the reaction of Ultraluminescence photometric determination, the suction of calculating
Attached amount result is shown in Fig. 4.The result shows that with the increase of initial concentration, adsorbance also increases.It is living when initial concentration is 8mg/L
Change montmorillonite biology carbon composite to the adsorbance maximum of estradiol and ethinyloestradiol up to 137 and 90mg/g.
Embodiment 4
A kind of method that the activation montmorillonite biology carbon composite of the present invention removes estrogen in water body, step and reality
The Adsorption for applying estrogen in 1 water body of example is identical, is different only in that：The pH value that solution is adjusted in embodiment 4 is 3.0-11.0.
The estrogen solution of a concentration of 6mg/L after taking 100mL to dilute adjusts solution with a concentration of 1M NaOH and HCl solution
PH value be 3.0,4.0,5.0,6.0,7.0,8.0,9.0,10.0 and 11.0, be added that 5mg embodiments 1 are obtained to activate montmorillonite
Biological carbon composite is placed in 25 DEG C of constant temperature oscillations, and water-bath constant temperature oscillator rotating speed is 170rpm, and duration of oscillation is for 24 hours, instead
Ying Hou, solution sedimentation, using 0.45 μm of Teflon filtration (syringe type).It is molten after being reacted with Ultraluminescence photometric determination
The adsorbance result of the concentration of estrogen in liquid, calculating is shown in Fig. 5.The result shows that pH activates montmorillonite charcoal 8.0 or so
Composite material reaches maximum to the adsorbance of estrogen.
Embodiment 5
A kind of method that the activation montmorillonite biology carbon composite of the present invention removes estrogen in water body, step and reality
The Adsorption for applying estrogen in 1 water body of example is identical, is different only in that：To the activation montmorillonite biology after absorption in embodiment 5
Carbon composite carries out 4 circular regenerations.
The activation montmorillonite life obtained of 5mg embodiments 1 is added in the estrogen solution of a concentration of 6mg/L after taking 100mL to dilute
Object carbon composite is placed in 25 DEG C of constant temperature oscillations, and water-bath constant temperature oscillator rotating speed is 170rpm, and duration of oscillation is reaction for 24 hours
Afterwards, solution settles, using 0.45 μm of Teflon filtration (syringe type).Solution after being reacted with Ultraluminescence photometric determination
The adsorbance result of the concentration of middle estrogen, calculating is shown in Fig. 6.The result shows that after 4 circular regenerations, montmorillonite is activated
Biological carbon composite still retains the adsorbance of estradiol and ethinyloestradiol the 82% and 69% of first adsorbance, illustrates that activation is covered
The cycling and reutilization of de- stone biology carbon composite is high.
As it can be seen that the present invention can efficiently remove estrogen in water body by using activation montmorillonite biology carbon composite.With
It is upper described, only it is presently preferred embodiments of the present invention, is not intended to limit the present invention in any form.Although the present invention is
It is disclosed as above with preferred embodiment, however, it is not intended to limit the invention.Any technical person familiar with the field is not departing from
In the case of the Spirit Essence and technical solution of the present invention, all using the methods and technical content of the disclosure above to skill of the present invention
Art scheme makes many possible changes and modifications, or is revised as the equivalent embodiment of equivalent variations.Therefore, every without departing from this
The content of inventive technique scheme, according to the technical essence of the invention it is made to the above embodiment it is any it is simple modification, equally replace
It changes, equivalence changes and modification, in the range of still falling within technical solution of the present invention protection.
Claims (7)
1. a kind of method of estrogen in montmorillonite biology carbon composite removal water body using activation, which is characterized in that including
Following steps：Montmorillonite and husk biomass are mixed into hydrothermal carbonization, KOH activation then is carried out to it；It is described obtain it is compound
Material completes the Adsorption to estrogen.
2. the method for estrogen in the montmorillonite biology carbon composite removal water according to claim 1 using activation,
It is characterized in that, the activation montmorillonite biology carbon composite is through the following steps that be prepared：
(1) montmorillonite and charcoal are mixed, is dissolved in 70mL ultra-pure waters, this suspension is placed in 100mL reaction kettles, in baking
Heating in dry case, it is cooling, then it is thoroughly washed repeatedly with deionized water, methanol washing by soaking filters, drying.
(2) KOH is added in montmorillonite biology carbon composite after drying in step (1) to activate, after being activated
Montmorillonite biology carbon composite.
3. the method for estrogen in the montmorillonite biology carbon composite removal water according to claim 2 using activation,
It is characterized in that, in the preparation process (1) of the activation montmorillonite biology carbon composite, the montmorillonite and charcoal mixing ratio
Example is 1:1, heating condition in the drying box：Temperature is 180 DEG C, time 16h.
4. the method for estrogen in the montmorillonite biology carbon composite removal water according to claim 2 using activation,
It is characterized in that, in the preparation process (2) of the activation montmorillonite biology carbon composite, KOH is added and montmorillonite charcoal is multiple
The ratio of condensation material is 1%, soak time 4h.
5. the method for estrogen in the montmorillonite biology carbon composite removal water according to claim 1 using activation,
It is characterized in that, the estrogen in the water body is two kinds, estradiol and female alkynol.
6. the method for estrogen in the montmorillonite biology carbon composite removal water according to claim 1 using activation,
It being characterized in that, the concentration control of estradiol and female alkynol in the water body is controlled in 0.2-8.0mg/L, pH in 3.0-11.0,
Temperature control is at 25 DEG C, rotating speed 170rpm.
7. the method for estrogen in the montmorillonite biology carbon composite removal water according to claim 1 using activation,
It is characterized in that, the equilibrium adsorption capacity of estradiol and female alkynol in the water body respectively reaches 114 and 69mg/g.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710303997.1A CN108786723A (en) | 2017-05-03 | 2017-05-03 | Utilize the method for estrogen in activation montmorillonite biology carbon composite removal water body |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624510A (en) * | 2019-09-11 | 2019-12-31 | 合肥学院 | Composite adsorbent and method for treating chrome black-containing T printing and dyeing wastewater by using same |
| CN111135795A (en) * | 2020-01-21 | 2020-05-12 | 温州子久堂生物科技有限公司 | Preparation method and application of adsorption material for gardenia essential oil head fragrance extraction |
| CN112892482A (en) * | 2021-01-26 | 2021-06-04 | 中国热带农业科学院海口实验站 | Preparation method of halloysite-biochar composite material |
| CN115025821A (en) * | 2022-06-17 | 2022-09-09 | 湖南农业大学 | Hydrothermal carbon composite material, preparation method thereof, catalytic system and application |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110624510A (en) * | 2019-09-11 | 2019-12-31 | 合肥学院 | Composite adsorbent and method for treating chrome black-containing T printing and dyeing wastewater by using same |
| CN110624510B (en) * | 2019-09-11 | 2021-10-29 | 合肥学院 | Composite adsorbent and method for treating chrome black-containing T printing and dyeing wastewater by using same |
| CN111135795A (en) * | 2020-01-21 | 2020-05-12 | 温州子久堂生物科技有限公司 | Preparation method and application of adsorption material for gardenia essential oil head fragrance extraction |
| CN112892482A (en) * | 2021-01-26 | 2021-06-04 | 中国热带农业科学院海口实验站 | Preparation method of halloysite-biochar composite material |
| CN112892482B (en) * | 2021-01-26 | 2023-03-17 | 中国热带农业科学院海口实验站 | Preparation method of halloysite-biochar composite material |
| CN115025821A (en) * | 2022-06-17 | 2022-09-09 | 湖南农业大学 | Hydrothermal carbon composite material, preparation method thereof, catalytic system and application |
| CN115025821B (en) * | 2022-06-17 | 2024-01-12 | 湖南农业大学 | Hydrothermal carbon composite material, preparation method thereof, catalytic system and application |
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Application publication date: 20181113 |