CN105344340A - Nonmetal carbon material catalyst, and preparation method and application thereof - Google Patents
Nonmetal carbon material catalyst, and preparation method and application thereof Download PDFInfo
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- CN105344340A CN105344340A CN201510655987.5A CN201510655987A CN105344340A CN 105344340 A CN105344340 A CN 105344340A CN 201510655987 A CN201510655987 A CN 201510655987A CN 105344340 A CN105344340 A CN 105344340A
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/37—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by reduction, e.g. hydrogenation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
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Abstract
The invention discloses a nonmetal carbon material catalyst. The catalyst is prepared through mixed dissolving of citric acid and primary amine hydrochloride according to a mol ratio of 1: (0.75-1.25) and a reaction at 160 to 200 DEG C for 2 min to 4 h. The catalyst can be used for catalyzing reductive degradation of dyes so as to treat dye waste water, overcomes the defects of complex preparation steps, high cost and proneness to secondary pollution of conventional metal nanometer catalysts, and has the advantages of good environmental compatibility, high catalysis efficiency, easy availability of raw materials, easiness and rapidness in preparation and suitability for large-scale production and practical application.
Description
Technical field
The present invention relates to a kind of catalyst field, be specifically related to a kind of non-metal carbon material catalyst and preparation method thereof and the application in degradation of dye.
Background technology
Dyestuff refers to the material that fiber can be made to obtain color and luster, is widely used in fields such as textile, leather, food, coating, ink and rubber always.Along with the fast development of society, a large amount of production of organic dyestuff and excessively use the water pollution problems caused, has developed into a global problem gradually, closely bound up with the productive life of the mankind.Dyestuff, in production and processing procedure, except utilizing water normally and processing, also has 12% to discharge with waste water formation.If waste water from dyestuff can not well process after discharge, be easy to directly cause earth's surface and underground water pollution, these water, once be drunk by animal and human, often bring irreversible injury.Meanwhile, organic dyestuff itself possesses gay colours usually, can effectively stop penetrating of light, the photosynthesis of severe jamming water plant.More seriously, organic dyestuff is mostly the material being difficult to degrade, can long-time stable be present in ecological environment, cause lasting pollution, the living environment of harm humans and healthy.
Traditional physical means, such as hyperfiltration, chemocoagulation, active carbon adsorption and ion exchange resin adsorb the dyestuff can effectively removed in water body.But these simple physics or chemiadsorption are only that pollutant is transferred to other phase, very easily cause secondary pollution.In addition, the post processing of sorbing material and the process of recycling very complicated, involve great expense.Therefore people begin one's study and may be used for the method for dye degrades.Research field is concentrated to be under natural daylight, utilize this type of dyestuff of titanium dioxide series catalyst photocatalytic degradation at present, but due to the band gap that titanium dioxide is wider, make this class catalyst only in specific apparatus and competence exertion effect under consuming the condition of a large amount of non-renewable energy resources simultaneously, and catalytic process is consuming time longer, makes it develop, apply and be greatly limited.Therefore, the method processing dyestuff simply, is fast and effectively set up extremely urgent.
At present, metal nano material catalysis dye degrades obtains the extensive concern of researcher.This kind of catalyst can the oxidation of catalysis dyestuff or reduction process, makes to reach degraded in its short time.Method is simple consuming time short.Although this kind of metal nano material possesses stronger catalytic effect, also there is obvious defect, as complicated time-consuming in prepared, easily occurring reunites reduces auto-catalytic activity, involves great expense, is unfavorable for producing widely and using simultaneously.In addition, metal nano material is in catalytic process, and can enter water body, removal process is loaded down with trivial details, if do not reclaim, can cause the secondary pollution of water body.Therefore, develop the nonmetal catalyzed nano material that can be used in catalysis dye degrades and possess significant advantage.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides a kind of non-metal carbon material catalyst and preparation method thereof and the application in degradation of dye.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of non-metal carbon material catalyst, by being 1:(0.75 ~ 1.25 in molar ratio by citric acid and primary amine hydrochloride) mixed dissolution, within 2 minutes ~ 4 hours, obtain in 160-200 DEG C of reaction, such material with carbon element is also referred to as carbon quantum dot at present.
Further, described primary amine hydrochloride is preferably C1-C18 kiber alkyl amine hydrochloride, and described C1-C18 kiber alkyl amine hydrochloride is preferably methylamine hydrochloride, ethylamine hydrochloride, ethylenediamine-hydrochloride and/or propylamin hydrochloride.
Further, described reaction adopts heating using microwave, reaction 2-10 minute.
Prepare a method for non-metal carbon material catalyst, comprise the steps: that by citric acid and primary amine hydrochloride be 1:(0.75 ~ 1.25 in molar ratio) mixed dissolution, in 160-200 DEG C of reaction 2 minutes ~ 4 hours, obtain described catalyst.
Preferably, by citric acid and primary amine hydrochloride mixed dissolution in water.
Above-mentioned non-metal carbon material catalyst is for the catalytic degradation of dyestuff or as embedded photoluminescent material.
Further, described dyestuff is methylene blue.
Further, described catalyst is degraded for the catalytic reduction of methylene blue.
Further, the catalytic reduction of the described methylene blue reducing agent adopted of degrading is hydrazine hydrate, and preferably, the concentration of described catalyst is 1-10 μ g/mL.
Beneficial effect of the present invention:
Instant invention overcomes the shortcoming of existing traditional metallic catalyst, such as preparation process is loaded down with trivial details, and cost is high, easily causes secondary pollution, is difficult to recycling etc.Novel metalloid carbon nanomaterial that the present invention adopts microwave method to prepare (this method prepare carbon nanomaterial be also referred to as carbon quantum dot at present) breaches tradition must have metal superlattice could be used for realizing the bottleneck of dyestuff catalytic degradation, overcome the defect of metal nano material, raw materials usedly to be easy to get, low price, be easy to a large amount of production and commercial introduction, the catalytic capability of the metal nano material of catalytic efficiency and report is suitable, without the need to illumination, degradation speed is fast, can implement under normal temperature, possesses good Environmental compatibility, without the need to the recycling of complexity after using, non-secondary pollution, green energy conservation.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for description, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is transmission electron microscope picture (a) and the XRD spectra (b) of catalyst of the present invention.
Fig. 2 is the fluorescence spectrum figure of catalyst of the present invention.
Fig. 3 is the uv-vis spectra variation diagram that after adding catalyst of the present invention, methylene blue catalytic reduction is degraded.
Fig. 4 is that methylene blue degradation rate is schemed over time.
Fig. 5 is the comparison diagram of the catalyst degradation of methylene blue ability that microwave method and hydro-thermal method prepare.
Fig. 6 is take Huanghe water as the degradation effect of medium methylene blue under catalyst reduction of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
embodiment 1
By 0.5g citric acid and 0.176g methylamine hydrochloride mixed dissolution in 10mL water, be placed in micro-wave oven (rated power 700W), microwave-heating 4 minutes (temperature is about 180 DEG C), cooled and filtered, washing, drying obtain black solid.
embodiment 2
By 0.5g citric acid and 0.268g ethylamine hydrochloride mixed dissolution in 10mL water, be placed in micro-wave oven, 4 minutes (temperature is about 180 DEG C) of microwave-heating, cooling, filter, washing, drying obtain black solid.
embodiment 3
By 0.5g citric acid and 0.201g ethylenediamine-hydrochloride mixed dissolution in 10mL water, be placed in micro-wave oven, 10 minutes (temperature is about 165 DEG C) of microwave-heating, cooling, filter, washing, drying obtain black solid.
embodiment 4
By 0.5g citric acid and 0.249g n-propylamine hydrochloride mixed dissolution in 10mL water, be placed in micro-wave oven, 2 minutes (temperature is about 200 DEG C) of microwave-heating, cooling, filter, washing, drying obtain black solid.
embodiment 5
By 0.5g citric acid and 0.176g methylamine hydrochloride mixed dissolution in 10mL water, transfer to the reactor that inner bag is polytetrafluoroethylene (PTFE), be placed in baking oven, heating temperatures most about 180 DEG C, react 3 hours, concentrated, filter, washing, drying obtain solid.
embodiment 6 methylene blue degradation experiment
As can be seen from transmission electron microscope picture (a) and the XRD spectra (b) of Fig. 1, the black solid size of gained of the present invention is at the particle of about 2nm, for non-metal carbon nano material, wherein carbon exists with amorphous carbon, the fluorescence spectrum of composition graphs 2 characterizes, under different excitation wavelength, the fluorescent emission signals of different wave length can be obtained, illustrate that this non-metal carbon nano material is carbon quantum dot.
As catalyst, catalytic degradation is carried out, for methylene blue to dyestuff using the black solid of embodiment 1 gained.Under normal temperature condition, join in methylene blue solution, then add appropriate catalyst by appropriate reducing agent hydrazine hydrate, wherein the concentration of system Methylene Blue is 0.03mmol/L, and the concentration of hydrazine hydrate is 0.09mol/L, and catalyst concn is 5.0 μ g/mL.
As shown in the uv-vis spectra of Fig. 3, add catalyst after 2 minutes uv-vis spectra sharply reduce, to almost disappearing, illustrates that methylene blue degraded is complete, its catalytic capability is suitable with metal nano material.
As shown in Figure 4, when not having catalyst, react after 30 minutes, the degradation rate of methylene blue less than 2%, and adds catalyst after 2 minutes, and degradation rate just reaches more than 99%.In addition, only having under methylene blue and catalyst (not adding reducing agent) existence condition, degrading, illustrating that fading of methylene is the absorption deriving from catalytic reduction effect instead of catalyst.As can be seen from Figure 5, the degradation rate of catalyst (embodiment 5) reaction methylene blue after 30 minutes prepared by hydro-thermal method only has about 20%, the material that material (embodiment 1) catalytic effect adopting microwave heating method to prepare is prepared far above hydro-thermal method is described, and adopts the preparation time of microwave method material can foreshorten to 2-10 minute by several hours.
Get Huanghe water as actual sample, and add methylene blue wherein, investigate catalyst feasibility in actual applications.As Fig. 6, add methylene blue and hydrazine hydrate in Huanghe water after, solution colour keeps blue constant, after adding catalyst, there is deoxidization, degradation rapidly in catalysis methylene blue, after 60 seconds, solution colour is thin out, after extra 30 seconds, color disappears substantially, illustrates that this method can use the degraded of actual sample Methylene Blue.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a non-metal carbon material catalyst, by being 1:(0.75 ~ 1.25 in molar ratio by citric acid and primary amine hydrochloride) mixed dissolution, within 2 minutes ~ 4 hours, obtain in 160-200 DEG C of reaction.
2. catalyst according to claim 1, it is characterized in that, described primary amine hydrochloride is preferably C1-C18 kiber alkyl amine hydrochloride, and described C1-C18 kiber alkyl amine hydrochloride is preferably methylamine hydrochloride, ethylamine hydrochloride, ethylenediamine-hydrochloride and/or propylamin hydrochloride.
3. catalyst according to claim 1, is characterized in that, described reaction adopts heating using microwave, reaction 2-10 minute.
4. prepare a method for non-metal carbon material catalyst, comprise the steps: that by citric acid and primary amine hydrochloride be 1:(0.75 ~ 1.25 in molar ratio) mixed dissolution, in 160-200 DEG C of reaction 2 minutes ~ 4 hours, obtain described catalyst.
5. preparation method according to claim 4, is characterized in that, by citric acid and primary amine hydrochloride mixed dissolution in water.
6. catalyst described in claim 1 is for the catalytic degradation of dyestuff or as embedded photoluminescent material.
7. application according to claim 6, described dyestuff is methylene blue.
8. application according to claim 7, is characterized in that, described catalyst is degraded for the catalytic reduction of methylene blue.
9. application according to claim 8, is characterized in that, the catalytic reduction of the described methylene blue reducing agent adopted of degrading is hydrazine hydrate.
10. application according to claim 9, is characterized in that, in catalytic reduction reaction system, the concentration of described catalyst is 1-10 μ g/mL.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106396176A (en) * | 2016-11-02 | 2017-02-15 | 赵青娇 | Dye printing sewage treatment method |
| CN106495358A (en) * | 2016-11-02 | 2017-03-15 | 赵青娇 | A kind of dye wastewater processing method |
| CN106517582A (en) * | 2016-11-25 | 2017-03-22 | 南宁市黑晶信息技术有限公司 | Method for treating printing and dyeing wastewater of pure wool textile fabrics |
| CN111537422A (en) * | 2020-06-10 | 2020-08-14 | 兰州大学 | Method for representing and regulating and controlling permeability in mushy zone during directional solidification of peritectic alloy |
| CN113388389A (en) * | 2021-07-23 | 2021-09-14 | 齐鲁工业大学 | Fluorescent carbon nanodot, preparation method and application thereof in cell nucleus targeted imaging |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106396176A (en) * | 2016-11-02 | 2017-02-15 | 赵青娇 | Dye printing sewage treatment method |
| CN106495358A (en) * | 2016-11-02 | 2017-03-15 | 赵青娇 | A kind of dye wastewater processing method |
| CN106517582A (en) * | 2016-11-25 | 2017-03-22 | 南宁市黑晶信息技术有限公司 | Method for treating printing and dyeing wastewater of pure wool textile fabrics |
| CN111537422A (en) * | 2020-06-10 | 2020-08-14 | 兰州大学 | Method for representing and regulating and controlling permeability in mushy zone during directional solidification of peritectic alloy |
| CN111537422B (en) * | 2020-06-10 | 2022-09-23 | 兰州大学 | Method for representing and regulating and controlling permeability in mushy zone during directional solidification of peritectic alloy |
| CN113388389A (en) * | 2021-07-23 | 2021-09-14 | 齐鲁工业大学 | Fluorescent carbon nanodot, preparation method and application thereof in cell nucleus targeted imaging |
| CN113388389B (en) * | 2021-07-23 | 2022-03-29 | 齐鲁工业大学 | Fluorescent carbon nanodot, preparation method and application thereof in cell nucleus targeted imaging |
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| CN105344340B (en) | 2018-01-26 |
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