CN109174003A - It is a kind of biology carbon composite preparation method and to estradiol removal application - Google Patents
It is a kind of biology carbon composite preparation method and to estradiol removal application Download PDFInfo
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- CN109174003A CN109174003A CN201811286141.9A CN201811286141A CN109174003A CN 109174003 A CN109174003 A CN 109174003A CN 201811286141 A CN201811286141 A CN 201811286141A CN 109174003 A CN109174003 A CN 109174003A
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- carbon composite
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- sodium hydroxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—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
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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
- B01J20/3021—Milling, crushing or grinding
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/305—Endocrine disruptive agents
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- Environmental & Geological Engineering (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Application the invention discloses a kind of preparation method for the biological carbon composite for belonging to technical field of environment function material preparation and to estradiol removal.This method is to add montmorillonite powder by the way that potassium hydroxide or sodium hydroxide is soluble in water, cow dung powder is added after ultrasonic disperse, then will lead to protection hermetic seal after mixed liquor ultrasonic disperse, dipping, heats and is cooled to room temperature after insulation reaction.Prepared biological carbon composite has large specific surface area, and surface has a variety of functional groups, and adsorption site is more, and adsorption capacity is stronger.
Description
Technical field
The invention belongs to technical field of environment function material preparation, in particular to a kind of preparation side of biological carbon composite
Method and the application that estradiol is removed.
Background technique
Non-steroidal estrogenic is a kind of incretion interferent, and autologous hormones effect, jammer can be simulated by entering in body
The synthesis of the endocrine substance of body, transhipment, metabolism, in conjunction with etc. processes.In recent years, in surface water, underground water, soils and sediments
In, non-steroidal estrogenic is detected extensively.Wherein, 17 beta estradiols are considered as estrogen effect in several environmental estrogens
Strongest one kind.The method of processing waste water containing estrogen has the methods of absorption, photocatalysis, biodegrade, and wherein absorption method is the most
Simply, economy and facility.Therefore, the adsorbent material for developing a kind of cost effective advantageously accounts for absorption method applied to wastewater treatment
The problem of.
Summary of the invention
Application the purpose of the present invention is to provide a kind of preparation method of biological carbon composite and to estradiol removal,
It is characterized in that, specific step is as follows:
(1) fresh cow dung is air-dried, is crushed, cross 0.25mm sieve；
(2) potassium hydroxide or sodium hydroxide for weighing 50-100g are dissolved in 1L water, then the montmorillonite powder of the quality such as addition
End, ultrasonic disperse 30-60min；
(3) the cow dung powder of 2 times of potassium hydroxide or sodium hydroxide quality is added, ultrasonic disperse 2-2.5h impregnates 16-
For 24 hours, it is then freeze-dried；
(4) sample after freeze-drying is placed in crucible, is put into Muffle furnace, is passed through in Muffle furnace close after protecting gas
Envelope is heated to predetermined temperature, keeps the temperature 2-3h, and after being cooled to room temperature, sample grinding is obtained charcoal composite material.
Wherein the step of (2) potassium hydroxide or the mass concentration of sodium hydroxide be 5-10wt%.
Wherein the step of (2), montmorillonite and the potassium hydroxide or the mass ratio of sodium hydroxide of being added was 1:1.
The cow dung of wherein the step of (3) described addition and the mass ratio of montmorillonite are 2:1.
The temperature of wherein the step of (3) described lyophilization is -45 DEG C, and the time of processing is 24-48h.
Wherein the step of (4) protection gas is one of nitrogen, carbon dioxide, helium, duration of ventilation 15-
20min。
Wherein the step of (4) heating rate is 5 DEG C/min, and scheduled temperature is 350-450 DEG C.
The biology carbon composite is applied to enhancing to the adsorption capacity of 17 beta estradiols.
The invention has the benefit that charcoal composite material and preparation method thereof proposed by the present invention is quick and easy, it is multiple to be not necessarily to
Miscellaneous instrument and equipment, raw materials used widely distributed, readily available, prepared composite material has nontoxic, specific surface area
Greatly, the feature more than surface functional group is high to the removal efficiency of 17 beta estradiols.
Detailed description of the invention
Fig. 1 is the scanning electron microscope structure chart of biological carbon composite in embodiment 1；
Fig. 2 is the adsorbance measurement result figure of reaction solution in embodiment 3；
Fig. 3 is the adsorbance measurement result figure of reaction solution in embodiment 4；
Fig. 4 is the adsorbance measurement result figure of reaction solution in embodiment 5.
Specific embodiment
Application the present invention provides a kind of preparation method of biological carbon composite and to estradiol removal, below with reference to
The present invention is described further for drawings and examples.
Embodiment 1:
Biological carbon composite specific the preparation method is as follows:
(1) fresh cow dung is air-dried, is crushed, cross 0.25mm sieve；
(2) potassium hydroxide for weighing 50g is dissolved in 1L water, and 50g montmorillonite powder, ultrasonic disperse 30min is added.
(3) the above-mentioned cow dung powder of 100g, ultrasonic disperse 2h is added, dipping is freeze-dried 48h at -45 DEG C for 24 hours, then.
(4) sample after freeze-drying is placed in crucible, is put into Muffle furnace, 15min nitrogen is passed through in Muffle furnace
After seal, be heated to 450 DEG C with 5 DEG C/min heating, keep the temperature 2h, after being cooled to room temperature, sample grinding is obtained into charcoal
Composite material.
Biology carbon composite appearance obtained above is black, places it under scanning electron microscope and observes, surface texture
As shown in Figure 1, being observed that the composite material surface is coarse by Fig. 1, there is pore structure abundant.
Embodiment 2:
Biological carbon composite prepared by embodiment 1 is applied to 17 beta estradiols of removal, and the specific method is as follows:
(1) compound concentration gradient is the 17 beta estradiol solution of 0.4-2.4mg/L.
(2) the biological carbon composite of 5mg is weighed into conical flask, the addition above-mentioned 17 beta estradiol solution of 50mL, 25 DEG C
Lower constant temperature oscillation 48h.
(3) it takes 2mL suspension to be centrifuged after adsorption equilibrium with the rate of 8000r/min, crosses 0.22 μm of glass filters
It is added in sample cell afterwards, solution concentration after being reacted using fluorescent spectrophotometer assay.The results are shown in Table 1:
Table 1: the adsorbance data under different 17 beta estradiol primary condition
| Initial concentration (mg/L) | Adsorbance (mg/g) |
| 2.4 | 10.95 |
| 2.0 | 11.24 |
| 1.6 | 9.49 |
| 1.2 | 6.84 |
| 0.8 | 1.29 |
| 0.4 | 0.80 |
As shown in Table 1, the biology carbon composite is to 17 beta estradiols adsorption capacity with higher, and with initial dense
Degree increases, adsorption capacity enhancing.
Embodiment 3:
Biological carbon composite prepared by embodiment 1 is applied to 17 beta estradiols of removal, and the specific method is as follows:
(1) the biological carbon composite of 10mg is weighed into conical flask, and the 2.4mg/L17 beta estradiol that 100mL is added is molten
Liquid, in 25 DEG C of constant temperature oscillation 48h.
(2) 0-1600min different interval time point (30,60,90,120,180,240,360,480,720,1080,
It 1440min) takes 1mL suspension to be centrifuged with 8000r/min, is added in sample cell after then crossing 0.22 μm of glass filters,
The levels of solution after being reacted with fluorescent spectrophotometer measuring.
Adsorbance result under different time is as shown in Fig. 2, as shown in Figure 2, the biology carbon composite female to 17 β-two
The adsorbance of alcohol is continuously increased as time increases.Between 0-120min, adsorbance is quicklyd increase, after 120min by
Gradually reach saturation.
Embodiment 4:
Biological carbon composite prepared by embodiment 1 is applied to 17 beta estradiols of removal, and the specific method is as follows:
(1) the biological carbon composite of 5 parts of 5mg is weighed into conical flask, and 17 β-for being separately added into 50mL 2.4mg/L are female
Glycol solution, while adjusting pH value with the NaOH and HCl of 0.1mol/L is 3,5,7,9,11, in 25 DEG C of constant temperature oscillation 48h.
(2) it takes 2mL suspension to be centrifuged after adsorption equilibrium with the rate of 8000r/min, crosses 0.22 μm of glass filters
It is added in sample cell afterwards, the solution concentration after being reacted with fluorescent spectrophotometer measuring.
Adsorbance result under different pH value is as shown in figure 3, from the figure 3, it may be seen that the adsorption effect of composite material is by pH value shadow
It rings, is unfavorable for removal of the adsorbent to 17 beta estradiols when pH value is higher, when pH value is 11, adsorbance is sharply reduced.
Embodiment 5:
Biological carbon composite prepared by embodiment 1 is applied to 17 beta estradiols of removal, and the specific method is as follows:
(1) the biological carbon composite of 5 parts of 5mg is weighed into conical flask, and 17 β-for being separately added into the 2.4mg/L of 50mL are female
Glycol solution, while the NaCl of different quality is added, make ionic strength 0,0.001,0.005,0.01,0.1mol/ of solution
L, in 25 DEG C of constant temperature oscillation 48h.
(2) it takes 2mL suspension to be centrifuged after adsorption equilibrium with the rate of 8000r/min, crosses 0.22 μm of glass filters
It is added in sample cell afterwards, the solution concentration after being reacted with fluorescent spectrophotometer measuring.
Adsorbance result under different ionic strength as shown in figure 4, as shown in Figure 4, the adsorption effect of composite material follow from
Sub- intensity is unrelated.
The above is only the preferred embodiment for the present invention, the scope of the present invention is not limited merely to above-described embodiment, with this
Various process programs of the inventive concept without substantial differences are in protection scope of the present invention.
Claims (8)
1. a kind of preparation method of biology carbon composite, which is characterized in that specific step is as follows:
(1) fresh cow dung is air-dried, is crushed, cross 0.25mm sieve；
(2) potassium hydroxide or sodium hydroxide for weighing 50-100g are dissolved in 1L water, then the montmorillonite powder of the quality such as addition,
Ultrasonic disperse 30-60min；
(3) the cow dung powder of 2 times of potassium hydroxide or sodium hydroxide quality is added, ultrasonic disperse 2-2.5h impregnates 16-24h, so
After be freeze-dried；
(4) sample after freeze-drying is placed in crucible, is put into Muffle furnace, sealed after protection gas is passed through in Muffle furnace,
It is heated to predetermined temperature, keeps the temperature 2-3h, after being cooled to room temperature, sample grinding is obtained into charcoal composite material.
2. a kind of preparation method of biological carbon composite according to claim 1, which is characterized in that step (2) described hydrogen
The mass concentration of potassium oxide or sodium hydroxide is 5-10wt%.
3. a kind of preparation method of biological carbon composite according to claim 1, which is characterized in that step (2) is described to be added
The mass ratio for entering montmorillonite and potassium hydroxide or sodium hydroxide is 1:1.
4. a kind of preparation method of biological carbon composite according to claim 1, which is characterized in that step (3) is described to be added
The mass ratio of the cow dung and montmorillonite that enter is 2:1.
5. a kind of preparation method of biological carbon composite according to claim 1, which is characterized in that step (3) described jelly
Dry temperature is -45 DEG C, and the time of processing is 24-48h.
6. a kind of preparation method of biological carbon composite according to claim 1, which is characterized in that step (4) described guarantor
Shield gas is one of nitrogen, carbon dioxide, helium, duration of ventilation 15-20min.
7. a kind of preparation method of biological carbon composite according to claim 1, which is characterized in that step (4) described liter
Warm rate is 5 DEG C/min, and scheduled temperature is 350-450 DEG C.
8. biology carbon composite described in claim 1-7 any claim, which is characterized in that the biology carbon composite
Applied to enhancing to the adsorption capacity of 17 beta estradiols.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811286141.9A CN109174003A (en) | 2018-10-31 | 2018-10-31 | It is a kind of biology carbon composite preparation method and to estradiol removal application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811286141.9A CN109174003A (en) | 2018-10-31 | 2018-10-31 | It is a kind of biology carbon composite preparation method and to estradiol removal application |
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| CN109174003A true CN109174003A (en) | 2019-01-11 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105921110A (en) * | 2016-06-02 | 2016-09-07 | 环境保护部华南环境科学研究所 | Preparation method and application of cow dung biological carbon |
| CN106334526A (en) * | 2016-11-24 | 2017-01-18 | 湖南大学 | Preparation and application of manganese dioxide modified charcoal for removing 17beta-estradiol in water |
| CN106512970A (en) * | 2016-11-24 | 2017-03-22 | 湖南大学 | Method for preparing montmorillonite/biochar composite material through one-step type carbonization activation and application of montmorillonite/biochar composite material |
| CN106693890A (en) * | 2016-12-13 | 2017-05-24 | 湖南大学 | Application of biochar adsorbent prepared from rice agricultural byproducts |
| CN106732375A (en) * | 2017-01-18 | 2017-05-31 | 湖南大学 | A kind of preparation method and applications of clay mineral modification biological charcoal |
-
2018
- 2018-10-31 CN CN201811286141.9A patent/CN109174003A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105921110A (en) * | 2016-06-02 | 2016-09-07 | 环境保护部华南环境科学研究所 | Preparation method and application of cow dung biological carbon |
| CN106334526A (en) * | 2016-11-24 | 2017-01-18 | 湖南大学 | Preparation and application of manganese dioxide modified charcoal for removing 17beta-estradiol in water |
| CN106512970A (en) * | 2016-11-24 | 2017-03-22 | 湖南大学 | Method for preparing montmorillonite/biochar composite material through one-step type carbonization activation and application of montmorillonite/biochar composite material |
| CN106693890A (en) * | 2016-12-13 | 2017-05-24 | 湖南大学 | Application of biochar adsorbent prepared from rice agricultural byproducts |
| CN106732375A (en) * | 2017-01-18 | 2017-05-31 | 湖南大学 | A kind of preparation method and applications of clay mineral modification biological charcoal |
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Application publication date: 20190111 |