CN108786832A - A kind of layered double hydroxide composite material and its preparation and application - Google Patents
A kind of layered double hydroxide composite material and its preparation and application Download PDFInfo
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- CN108786832A CN108786832A CN201810601361.XA CN201810601361A CN108786832A CN 108786832 A CN108786832 A CN 108786832A CN 201810601361 A CN201810601361 A CN 201810601361A CN 108786832 A CN108786832 A CN 108786832A
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/86—Chromium
- B01J23/868—Chromium copper and chromium
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2101/308—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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/40—Organic compounds containing sulfur
Abstract
The present invention relates to a kind of layered double hydroxide composite material and its preparation and application, the composite material prepares hydro-thermal charcoal by raw material of biomass first, layered composite metal hydroxides are carried on by hydro-thermal carbon surface by hydrothermal synthesis method again, after being simply separated by solid-liquid separation, washing, dry.Hydro-thermal charcoal/layered double hydroxide composite material the energy and H that the method for the present invention obtains2O2Class Fenton's reaction system is formed, achievees the purpose that the pollutants such as water environment Chinese medicine object and personal-care supplies, incretion interferent, organic dyestuff of effectively degrading.Hydro-thermal charcoal/layered double hydroxide composite material is prepared simply, and reaction condition is mild, and utilization ratio is high, at low cost, is a kind of composite catalyst that application potential is larger.
Description
Technical field
The present invention relates to technology of waste water control fields, and in particular to a kind of layered double hydroxide composite material and its
Preparation and application.
Background technology
The emerging pollutant such as incretion interferent, drug and personal care articles causes extensive concern in recent years, due to its tool
There is hydrophobicity feature to be easy to be enriched in vivo, to disturb the normal physiology work(of organism in environment to a certain extent
Energy.It is emerging organic dirt of g/L grades of ng/L- μ that the earth's surface and groundwater environment of current many countries and regions, which have concentrations,
Object is contaminated, while the prior art that drinking water plant uses is limited to the treatment effect of this pollutant, in some instances it may even be possible to generate other pairs
Product and directly or indirectly influence health.Effective depth is also lacked to the related wastewater treatment of this pollutant simultaneously
Reason technology.
In recent years, comparatively fast developed with generating the advanced catalytic oxidation technology based on strong oxidizing property free radical, it is main
It is to attack organic pollution using living radical, organic molecule is gradually degraded as small-molecule substance, reaching efficiently removal has
The purpose of malicious harmful organic contaminants.Compared to being generated in conventional homogeneous Fenton's reaction there are pH response ranges narrow, reaction process
Iron cement and the problem of cannot achieve active component, the catalysis of multiphase-fenton Fenton have easy to operate, and reaction condition is mild, cost phase
To it is relatively low the features such as.However the class fenton catalyst to grow up at present deposit in neutral conditions it is active it is relatively low, stability is poor,
H2O2The deficiencies of utilization rate is relatively low.It is therefore desirable to be directed to prior art problem further to develop feasible method.
Layered double hydroxide (LDHs) due to its structure composition diversity, laminate metal ion high dispersion with
And the interchangeability of interlayer anion, it is with a wide range of applications in fields such as absorption, catalysis, environmental protection, energy reserves.
Different transition metal ions especially is introduced in the unique veneer structures of LDHs, LDHs can be made to live with good catalysis
Property, realize and H2O2The Fenton-like of composition is under pH neutrallty conditions to the degradation of organic pollution.But LDHs materials there is also
Deficiency is such as easy to reunite, and activated centre number is reduced etc..
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of activity is strong, prepares letter
Single layered double hydroxide composite material and its preparation and application.
The purpose of the present invention can be achieved through the following technical solutions：A kind of layered double hydroxide composite wood
Material, the material include the layered double hydroxide (LDH) being made of Kocide SD and chromium hydroxide and are supported on stratiform
The mass ratio of the hydro-thermal charcoal (HBC) on double-metal hydroxide surface, the hydro-thermal charcoal and layered double hydroxide is (0.01
~0.1)：1.The present invention not only has good catalytic activity by introducing hydro-thermal charcoal in layered double hydroxide, and
And hydro-thermal charcoal can effectively prevent the reunion of layered double hydroxide, improve the utilization rate of layered double hydroxide；
In addition, hydro-thermal carbon surface has abundant oxygen-containing functional group, the catalysis of layered double hydroxide can be further increased
Activity.
The molar ratio of Kocide SD and chromium hydroxide is 1 in the layered double hydroxide：(0.2~1).
A kind of preparation method of layered double hydroxide composite material as described above, includes the following steps：
(1) powdered biomass material is placed in water, obtains hydro-thermal charcoal under hydro-thermal reaction after mixing；
(2) by mantoquita and chromic salts it is soluble in water and it is uniformly mixed obtain mixed solution, alkaline reagent is added dropwise, and simultaneously by water
Hot charcoal is immersed in mixed solution, and stirring is subsequently placed in reaction kettle and reacts, and is filtered, washed, is drying to obtain layered double gold
Belong to hydroxide composite material.
The powdered biomass material is by agriculture and forestry product and waste through mechanical grinding grinds, washing, drying
It obtains；
The condition of the hydro-thermal reaction is：100~120 DEG C of temperature, the time 2~for 24 hours, the production that the hydro-thermal reaction obtains
Object is obtained through suction filtration mode, and is washed to neutrality, then dry under the conditions of 50~100 DEG C.
The mantoquita includes copper nitrate, copper chloride or copper sulphate, and the chromic salts includes chromic nitrate, chromium chloride or sulfuric acid
The molar ratio of chromium, the mantoquita and chromic salts is 1：(0.2~2).
The alkaline reagent is sodium hydroxide or potassium hydroxide.The additive amount of alkaline reagent is with completely by mantoquita and chromic salts
Conversion hydrate is preferred.
The hydro-thermal charcoal is immersed in mixed solution, stirs 0.5~4h.
Reaction temperature is 100~120 DEG C in the reaction kettle, and the reaction time is 8~15h, obtained product filtering, warp
Water washing, it is dry at a temperature of 40~70 DEG C, obtain layered double hydroxide composite material.In a kettle, hydro-thermal charcoal
A kind of nucleocapsid structure is showed, a large amount of metastable oxygen-containing functional groups is generated, is formed through hydro-thermal carbon and layered hydroxide
Combined processing, both can play respective comprehensive advantage, improve the utilization ratio of LDH, and generate certain synergistic effect, from
And improve the absorption degradation performance to organic pollution.
A kind of application of layered double hydroxide composite material as described above, the composite material and H2O2Mixing, so
It is added into the treatment sewage containing organic pollution, uniform stirring at a temperature of higher than 25 DEG C, is completed to having in sewage afterwards
The degradation of machine pollutant, wherein the dosage of the composite material is 0.01~10g/L, H2O2Dosage be 1~100mmol/L.
Since hydro-thermal carbon surface has the oxygen-containing functional groups such as abundant hydroxyl, carboxyl, carbonyl, and in hydro-thermal carbonization process
Middle generation persistent free radicals, at the same with layered double-hydroxide it is compound after, by laminate metal ion, further can efficiently live
Change H2O2, form the hydroxyl radical free radical of strong oxidizing property, and then catalytic degradation organic pollution.
The organic pollution includes organic dyestuff, incretion interferent, drug or personal-care supplies.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects：
(1) the hydro-thermal charcoal material surface used is containing the oxygen-containing functional group such as abundant hydroxyl, carboxyl, carbonyl, and in hydro-thermal
Generate persistent free radicals in carbonization process, at the same with layered double-hydroxide it is compound after, can be into one by laminate metal ion
Step efficiently activates H2O2, form the hydroxyl radical free radical of strong oxidizing property, and then catalytic degradation organic pollution；
(2) composite material of the invention utilizes hydrothermal synthesis method, prepares simply, synthesis condition is mild, and the former material utilized
Material environmental protection, advantage of lower cost；
(3) composite material and H of the invention2O2The class Fenton's reaction system of composition can reduce pH value of solution to treatment effect
It significantly affects, has evaded the problem that pH range accommodations are narrow in traditional Fenton's reaction.
Description of the drawings
Fig. 1 is the XRD diffraction schematic diagrames of CuCr-LDH in the embodiment of the present invention 1, HBC and its composite material；
Fig. 2 is the absorption and drop of CuCr-LDH, HBC and its composite material to sulfadimidine in the embodiment of the present invention 2
Solve kinetic test result；
Fig. 3 is that CuCr-LDH, HBC and its composite material are dynamic to the absorption and degradation of rhodamine B in the embodiment of the present invention 4
Mechanical test results.
Specific implementation mode
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention
Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of hydro-thermal charcoal/layered double hydroxide composite material of the present invention, specific preparation method include
Following steps：
(1) 9g biomass wood powder raw materials are put into after washing and drying in autoclave, and it is mixed that 75mL ultra-pure waters are added
It closes uniform.Reaction kettle is stablized under the conditions of 180 DEG C keeps 18h, and after being cooled to room temperature, through filtering, washing obtains water after dry
Hot charcoal.
(2) 30mL Cu containing 500mmol/L are prepared2+Solution A and 15mL Cr containing 250mmol/L3+Solution B, it is another to prepare
The solution C of 10mL NaOH containing 1000mmol/L.Above-mentioned prepared solution A is added in solution B, while being slowly added dropwise molten
In liquid C to above-mentioned mixed liquor, and 1%, 5% and 10% mass ratio hydro-thermal charcoal is added, through magnetic agitation 1h to ensure to have reacted
Entirely.
(3) reaction solution obtained is subsequently moved in hydrothermal reaction kettle heats 12h at 120 DEG C, is filtered and is divided by solid-liquid
From after, milli-Q water value neutrality, being dried at 60 DEG C to get to hydro-thermal charcoal/layered double hydroxide composite material.
The above-mentioned hydro-thermal charcoal being prepared/layered double hydroxide composite material appearance is dark green powder.Its XRD
(see Fig. 1) diffraction maximum has the characteristic diffraction peak of layered double hydroxide and hydro-thermal charcoal concurrently, illustrates LDH in hydro-thermal carbon surface
Compound action.
Embodiment 2
A kind of hydro-thermal charcoal/layered double hydroxide composite material is for removing water environment Chinese medicine species pollutant sulfanilamide (SN)
Diformazan pyrimidine, includes the following steps：
It is prepared through dilution using the storing solution of 500mg/L and obtains a concentration of 5mg/L sulfadimidines, take 100mL respectively
In conical flask.Hydro-thermal charcoal/layered double hydroxide the composite material prepared in adding 0.5g/L embodiments one it is same
When, the H that concentration of volume percent is 30% is added2O2Solution 2mL is placed under the conditions of being protected from light uniform stirring in constant temperature oscillator, drop
It is 25 DEG C to solve controlling reaction temperature in processing procedure, and according to certain time interval to the processing water after class Fenton's reaction
It is sampled, after 0.22 μm of membrane filtration, the residue using solution after ultra performance liquid chromatography (UPLC) analysis reaction is dense
Degree.Fig. 2 the result shows that, the removal rate of sulfadimidine reaches 80% or more after 0.5h, continue thereafter with reaction 5h, reach UPLC
It is not detected, close to 100% removal.The initial pH that sulfadimidine solution is handled in the present embodiment is 7.1, and hydro-thermal
The removal rate of charcoal/layered double hydroxide composite material is higher than the Fenton-like of single hydro-thermal charcoal and LDH, illustrates in
Property under the conditions of, can be with H through hydro-thermal charcoal and catalysis material compound LDH2O2Form Fenton-like degradation drug class sulfanilamide (SN) diformazan
Pyrimidine pollutant, and there is higher removal effect.
Embodiment 3
A kind of hydro-thermal charcoal/layered double hydroxide composite material is for removing incretion interferent in water environment female three
Alcohol includes the following steps：
It is prepared through dilution using the storing solution of 500mg/L and obtains a concentration of 2mg/L estriol, take 100mL in taper respectively
In bottle.While the hydro-thermal charcoal/layered double hydroxide composite material prepared in adding 0.5g/L embodiments one, it is added
The H that concentration of volume percent is 30%2O2Solution 2mL is placed under the conditions of being protected from light uniform stirring in constant temperature oscillator, degradation treatment
Controlling reaction temperature is 25 DEG C in the process, and is taken to the processing water after class Fenton's reaction according to certain time interval
Sample, after 0.22 μm of membrane filtration, using the residual concentration of solution after ultra performance liquid chromatography (UPLC) analysis reaction.As a result
60%, and the removal rate of hydro-thermal charcoal/layered double hydroxide composite material are reached to the degradation rate of estriol after showing 6h
It is substantially better than the Fenton-like of single hydro-thermal charcoal and LDH.The initial pH of estriol is 6.7 in the present embodiment, is illustrated through hydro-thermal
Charcoal and compound LDH catalysis material and H2O2The Fenton-like of the composition incretion interferent that can degrade to a certain extent is female
Triol, realization make full use of Fenton-like.
Embodiment 4
A kind of hydro-thermal charcoal/layered double hydroxide composite material for removing organic dyestuff rhodamine B in water environment,
Include the following steps：
It is prepared through dilution using the storing solution of 1000mg/L and obtains a concentration of 10mg/L rhodamine Bs, take 100mL in cone respectively
In shape bottle.While the hydro-thermal charcoal/layered double hydroxide composite material prepared in adding 0.5g/L embodiments one, add
Enter the H that concentration of volume percent is 30%2O2Solution 2mL, is placed under the conditions of being protected from light uniform stirring in constant temperature oscillator, at degradation
Controlling reaction temperature is 25 DEG C during reason, and is carried out to the processing water after class Fenton's reaction according to certain time interval
Sampling, after 0.45 μm of membrane filtration, using the residual concentration of solution after ultraviolet-uisible spectrophotometer analysis reaction.Fig. 3
The result shows that reaching 95% or more, and hydro-thermal charcoal/layered double hydroxide composite wood to the degradation rate of rhodamine B after 4h
The removal rate of material is substantially better than the Fenton-like of single hydro-thermal charcoal and LDH, illustrates through hydro-thermal charcoal and catalysis material compound LDH
With H2O2The Fenton-like of composition can degradating organic dye rhodamine B within a certain period of time, and there is higher removal rate.
Embodiment 5
Using preparation method similar to Example 1, the difference is that：
(1) molar ratio of copper nitrate and chromic nitrate is 1:0.2；
(2) mass ratio of hydro-thermal charcoal and hydroxide is 0.01:1；
(3) it is 0.5h that hydro-thermal charcoal, which is immersed in the mixing time in mixed solution,；Reaction temperature is 120 DEG C in reaction kettle, instead
It is 8h between seasonable, obtained product filtering is dry at a temperature of 40 DEG C through water washing.
By obtained composite material and H2O2The Fenton-like of composition being capable of degradating organic dye Luo Dan within a certain period of time
Bright B, and there is higher removal rate.
Embodiment 6
Using preparation method similar to Example 1, the difference is that：
(1) molar ratio of copper nitrate and chromic nitrate is 1:1；
(2) mass ratio of hydro-thermal charcoal and hydroxide is 0.1:1；
(3) it is 4h that hydro-thermal charcoal, which is immersed in the mixing time in mixed solution,；Reaction temperature is 100 DEG C in reaction kettle, reaction
Time is 15h, obtained product filtering, dry at a temperature of 70 DEG C through water washing.
By obtained composite material and H2O2The Fenton-like of composition being capable of degradating organic dye Luo Dan within a certain period of time
Bright B, and there is higher removal rate.
Claims (10)
1. a kind of layered double hydroxide composite material, which is characterized in that the material includes by Kocide SD and hydroxide
The layered double hydroxide of chromium composition and the hydro-thermal charcoal for being supported on layered double hydroxide surface, the hydro-thermal charcoal
Mass ratio with layered double hydroxide is (0.01~0.1)：1.
2. a kind of layered double hydroxide composite material according to claim 1, which is characterized in that the stratiform
The molar ratio of Kocide SD and chromium hydroxide is 1 in double-metal hydroxide：(0.2~1).
3. a kind of preparation method of layered double hydroxide composite material as claimed in claim 1 or 2, which is characterized in that
Include the following steps：
(1) powdered biomass material is placed in water, obtains hydro-thermal charcoal under hydro-thermal reaction after mixing；
(2) by mantoquita and chromic salts it is soluble in water and it is uniformly mixed obtain mixed solution, alkaline reagent is added dropwise, and simultaneously by hydro-thermal charcoal
It is immersed in mixed solution, stirs, be subsequently placed in reaction kettle and react, be filtered, washed, be drying to obtain layered bimetallic hydrogen
Oxide composite.
4. a kind of preparation method of layered double hydroxide composite material according to claim 3, which is characterized in that
The powdered biomass material is that agriculture and forestry product and waste are washed, are dried to obtain through mechanical grinding grinds；
The condition of the hydro-thermal reaction is：100~120 DEG C of temperature, the time 2~for 24 hours, the product warp that the hydro-thermal reaction obtains
Suction filtration mode obtains, and washs to neutrality, then dry under the conditions of 50~100 DEG C.
5. a kind of preparation method of layered double hydroxide composite material according to claim 3, which is characterized in that
The mantoquita includes copper nitrate, copper chloride or copper sulphate, and the chromic salts includes chromic nitrate, chromium chloride or chromium sulfate, the copper
The molar ratio of salt and chromic salts is 1：(0.2~2).
6. a kind of preparation method of layered double hydroxide composite material according to claim 3, which is characterized in that
The alkaline reagent is sodium hydroxide or potassium hydroxide.
7. a kind of preparation method of layered double hydroxide composite material according to claim 3, which is characterized in that
The hydro-thermal charcoal is immersed in mixed solution, stirs 0.5~4h.
8. a kind of preparation method of layered double hydroxide composite material according to claim 3, which is characterized in that
Reaction temperature is 100~120 DEG C in the reaction kettle, and the reaction time is 8~15h, obtained product filtering, through water washing,
It is dry at a temperature of 40~70 DEG C, obtain layered double hydroxide composite material.
9. a kind of application of layered double hydroxide composite material as claimed in claim 1 or 2, which is characterized in that described
Composite material and H2O2Then mixing is added into the treatment sewage containing organic pollution, at a temperature of higher than 25 DEG C uniformly
The degradation to dirty organic pollutants is completed in stirring, wherein the dosage of the composite material is 0.01~10g/L, H2O2's
Dosage is 1~100mmol/L.
10. a kind of application of layered double hydroxide composite material according to claim 9, which is characterized in that institute
The organic pollution stated includes organic dyestuff, incretion interferent, drug or personal-care supplies.
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| CN110433805A (en) * | 2019-08-22 | 2019-11-12 | 华南理工大学 | A kind of anionic clay-hydro-thermal charcoal sustained release photochemical catalytic oxidation material and the preparation method and application thereof |
| CN110433805B (en) * | 2019-08-22 | 2021-11-02 | 华南理工大学 | Anionic clay-hydrothermal carbon slow-release photocatalytic oxidation material and preparation method and application thereof |
| CN110586114A (en) * | 2019-09-19 | 2019-12-20 | 天津大学 | Preparation method of copper-chromium-aluminum hydrotalcite catalyst and application of catalyst in catalytic oxidation of 5-hydroxymethylfurfural |
| CN112142167A (en) * | 2020-09-07 | 2020-12-29 | 南京智汇环境气象产业研究院有限公司 | Preparation method of layered double-metal hydroxide Co-Fe-LDH electro-catalytic Fenton reaction cathode plate |
| CN112919752A (en) * | 2020-12-08 | 2021-06-08 | 金风环保有限公司 | Method for preparing sludge treatment agent and method for treating sludge |
| CN113401876A (en) * | 2021-07-05 | 2021-09-17 | 中山大学 | Method for producing hydrogen peroxide through photocatalysis without sacrificial agent |
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