CN106669596A - Preparation of CNX modified diatomite and method for taking advantage of CNX modified diatomite to adsorb Congo red waste water - Google Patents

Preparation of CNX modified diatomite and method for taking advantage of CNX modified diatomite to adsorb Congo red waste water Download PDF

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Publication number
CN106669596A
CN106669596A CN201710011256.6A CN201710011256A CN106669596A CN 106669596 A CN106669596 A CN 106669596A CN 201710011256 A CN201710011256 A CN 201710011256A CN 106669596 A CN106669596 A CN 106669596A
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composite material
congo red
diatomite composite
cnx
load
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CN106669596B (en
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王金淑
张大业
吴俊书
杜玉成
李洪义
贾新建
腾威利
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Beijing University of Technology
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Beijing University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28023Fibres or filaments
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention provides preparation of CNX modified diatomite and a method for taking advantage of the CNX modified diatomite to adsorb Congo red waste water, belonging to the technical field of waste water absorption. Melamine and diatomite are added into a reactor, the melamine and the diatomite are arranged in a water bath kettle at the temperature of 60-90 DEG C for dissolution, after the melamine is completely dissolved, nitric acid is diluted, the ratio of melamine mass to diatomite mass to a dilute nitric acid volume is (1-5g):(0.5-3g):10ml, the prepared solution is stirred in the water bath kettle for 10-30min, then, the solution is taken out to cool in air, after the solution takes the shape of a solid cotton fiber, filtration is taken out, and after the filtration, the solid is dried to obtain a CNX loaded diatomite composite material. Heat treatment is conducted further. The CNX modified diatomite is used as an adsorbent to adsorb a Congo red dye.

Description

CNXThe preparation of modification infusorial earth and the method for adsorbing Congo red waste water using it
Technical field
The invention belongs to waste water adsorption technology field, more particularly to adsorbent, prepare and using its process Congo red waste water Method.
Background technology
In recent years, dyestuff and heavy metal become the pith of environmental pollution.Dyestuff is a kind of important chemical products, it Have a wide range of applications, but the discharge of waste water from dyestuff can cause huge pollution to environment.The dyestuff of low concentration also can be produced very Dense color, to the healthy unfavorable of people.Further, since dyestuff reduces sunlight morning transmission in water, therefore, it can also shadow The growth of Xiangshui County plant.Wherein, Congo red is a kind of typical organic dyestuff.
At present waste water mainly has three kinds of processing methods, respectively physical action, chemical decomposition method and biological decomposition method.Tool Body method has absorption, extraction, ion exchange, electrodialysis, reverse osmosiss, Electrocatalytic Oxidation etc., and these methods can be successfully real The industrialization of existing wastewater treatment, but operating process is all more complicated, it could even be possible to causing secondary pollution so that the place of waste water Reason difficulty is increased.And absorption method is the ability for having selective absorption to certain component in liquid or gas using adsorbent so as to On the sorbent, so as to realize that the purpose of the component is separated from mixture, the process operation is safe and simple, nothing two for temporary deposition Secondary pollution.Wherein, activated carbon presents in the treatment of waste water good performance, but expensive.
To sum up, Handling Waste Water by Absorbing Way still has very big advantage in prior art, and during Handling Waste Water by Absorbing Way Still end reaches preferable effect to the adsorbent for being used, and the research and development of the adsorbent of excellent performance remain the current technical field section Grind the focus and difficult point of work.
The content of the invention
Present invention aims to the existing deficiency processed in Congo red waste water, there is provided a kind of efficiently to remove the Congo The adsorbent of red waste water, preparation method and process CN using itXThe method of load diatomite composite material waste water.
The purpose of the present invention is achieved through the following technical solutions:
CNXThe preparation method of load diatomite composite material, concretely comprises the following steps:Tripolycyanamide, kieselguhr are added into reaction It is placed in being dissolved in 60-90 DEG C of water-bath in device, dust technology, the matter of tripolycyanamide is added after tripolycyanamide is completely dissolved Measure and be respectively 1-5g with the bulking value of diatomaceous quality and nitric acid:0.5-3g:10ml (preferred 1g:1g:10ml), above-mentioned preparation Good solution, continues, in water-bath stirring, to stir 10-30min, then, takes out above-mentioned solution and is cooled down in atmosphere, treats shape Into after solid flocculence, filtered.Solid is dried after filtration, you can obtain CNXLoad diatomite composite material.
Dust technology concentration is conventional, and generally mass fraction is 2-6%.
Further preferably, to CN obtained aboveXThe further heat treatment calcining of load diatomite composite material, heat treatment bar Part is that under air conditionses, heat treatment temperature is 150-550 DEG C (preferred 150-250 DEG C), and the time 1-3 hour of heat treatment is excellent Select 2 hours.
By such scheme, after described drying terminates, the flocculence sample from color or Lycoperdon polymorphum Vitt is obtained.CNXLoad kieselguhr Composite, preferably its microscopic appearance are that fiber is bar-shaped, wherein, preferred CNXIt is 1-5 with diatomaceous mass ratio.
CNXFor carbon nitrogen organic material.
CNXLoad diatomite composite material is preferred for adsorbing congo red as the application of adsorbent.
One kind utilizes above-mentioned CNXThe method that load diatomite composite material processes congo red waste water, its concrete steps For:By CNXLoad diatomite composite material is added in the waste water containing congo red, is mixed and is stirred, and makes CNXLoad silicon Diatomaceous earth composite fully adsorbs Congo red, is then separated by filtration, and removing is adsorbed with the CN of Congo redXLoad composite diatomite material Material.
By such scheme, the initial concentration of Congo red waste water solution is 2000mg/L, is added in every 50mL Congo red solution Adsorbent amount be 0.1-0.5g;The concussion adsorption conditionses:30-50 DEG C of adsorption temp, concussion adsorption time is 1-5min, PH value is 6-7.
Beneficial effects of the present invention:
Compared with prior art, it is an advantage of the current invention that:
(1) adsorbent that the present invention is provided has higher specific surface area and relatively low cost, and environmental friendliness, neutral Or under solutions of weak acidity have good stability the features such as.
(2) CN that the present invention passes through the compound appropriate amount in kieselguhr matrixXFormed with for the bar-shaped CN of fiberXIt is negative Diatomite composite material is carried, the performance of its Adsorption Congo red can be obviously improved, reach the purpose of efficient removal.The composite wood Material 5min can reach adsorption equilibrium, and Congo red maximal absorptive capacity is up to 350mg/g.
(3) CN that the present invention is providedXLoad diatomite composite material adsorbent removes the method for waste water to be had without the need for special Equipment, step is simple and efficient, will not introduce other harmful substances in processing procedure, and the rate of adsorption is fast, the features such as adsorption efficiency is high.
Description of the drawings
Fig. 1 loads the field emission scanning electron microscope photo of diatomite composite material for the CNX of different heat treatment Temperature Treatment.
Fig. 2 loads the XRD of diatomite composite material for the CNX of different heat treatment Temperature Treatment
Fig. 3 is the infrared spectrogram before and after the absorption Congo red for measuring.
The adsorption time of adsorbents of the Fig. 4 obtained by a temperature of different heat treatment in the process example of congo red waste water With the graph of relation of C/C0.
The nonheat-treated CN of Fig. 5XThe Congo red of-diatomite adsorption variable concentrations.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.Following examples be merely to illustrate the present invention and without In restriction the scope of the present invention;It should be pointed out that after the content for having read instruction of the present invention, those skilled in the art can To make various changes or modifications to the present invention, these equivalent form of values equally fall within the model that the application appended claims are limited Enclose.Nitric acid mass fraction in following examples is 6%.
Embodiment 1
Step one, in mass ratio 1:1 adds tripolycyanamide and kieselguhr in beaker (open systemss), is subsequently adding certain The dust technology of amount, wherein kieselguhr are (1g with the mass volume ratio of nitric acid:10ml), 70 DEG C of beaker temperature, mixing speed are controlled For 120rpm, after reaction 1h, filter, take filtrate, be placed in drying baker and be dried.
Step 2, the filtrate being dried to obtain is positioned in crucible, is placed in Muffle furnace and is calcined 2 hours, calcining heat 150 DEG C, that is, CN is obtainedXLoad diatomite composite material.
Step 3, takes CNXLoad diatomite composite material 0.1g is added in concentration 2000mg/L Congo red 20ml, room temperature Ultrasonic disperse 2min, makes CNXLoad diatomite composite material is uniformly dispersed, and fully reacts with Congo red molecules.Reaction terminates Afterwards, by the reacting liquid filtering for obtaining separate, the Congo red waste water after adsorb and adsorb Congo red after CNXLoad kieselguhr Composite.
Implementation result:The CN that the present embodiment is preparedXLoad diatomite composite material, Congo red adsorbance is 321mg/ g。
Embodiment 2
Step one, in mass ratio 1:1.5 add kieselguhr and kieselguhr in beaker (open systemss), are subsequently adding certain The nitric acid of amount, wherein kieselguhr are (1g with the mass volume ratio of nitric acid:10ml), 70 DEG C of beaker temperature is controlled, mixing speed is 120rpm, after reaction 1h, filters, and takes filtrate, is placed in drying baker and is dried.
Step 2, the filtrate being dried to obtain is positioned in crucible, is placed in Muffle furnace and is calcined 2 hours, calcining heat 150 DEG C, that is, CN is obtainedXLoad diatomite composite material.
Step 3, takes CNXLoad diatomite composite material 0.1g is added in concentration 2000mg/L Congo red 20ml, room temperature Ultrasonic disperse 2min, makes CNXLoad diatomite composite material is uniformly dispersed, and fully reacts with Congo red molecules.Reaction terminates Afterwards, by the reacting liquid filtering for obtaining separate, the Congo red waste water after adsorb and adsorb Congo red after CNXLoad kieselguhr Composite.
Implementation result:The CN that the present embodiment is preparedXLoad diatomite composite material, Congo red adsorbance is 341mg/ g。
Embodiment 3
Step one, in mass ratio 1:2 add kieselguhr and kieselguhr in beaker (open systemss), are subsequently adding a certain amount of Nitric acid, the wherein mass volume ratio of kieselguhr and nitric acid is (2g:10ml), 70 DEG C of beaker temperature is controlled, mixing speed is 120rpm, after reaction 1h, filters, and takes filtrate, is placed in drying baker and is dried.
Step 2, the filtrate being dried to obtain is positioned in crucible, is placed in Muffle furnace and is calcined 2 hours, calcining heat 250 DEG C, that is, CN is obtainedXLoad diatomite composite material.
Step 3, takes CNXLoad diatomite composite material 0.1g is added in concentration 2000mg/L Congo red 20ml, room temperature Ultrasonic disperse 2min, makes CNXLoad diatomite composite material is uniformly dispersed, and fully reacts with Congo red molecules.Reaction terminates Afterwards, by the reacting liquid filtering for obtaining separate, the Congo red waste water after adsorb and adsorb Congo red after CNXLoad kieselguhr Composite.
Implementation result:The CN that the present embodiment is preparedXLoad diatomite composite material, Congo red adsorbance is 318mg/ g。

Claims (10)

1.CNXThe preparation method of load diatomite composite material, it is characterised in that concrete steps include as follows:By tripolycyanamide, Kieselguhr adds and is placed in being dissolved in 60-90 DEG C of water-bath in reactor, and dilute nitre is added after tripolycyanamide is completely dissolved The bulking value ratio of acid, the quality of tripolycyanamide and diatomaceous quality and dust technology is 1-5g:0.5-3g:10ml, it is above-mentioned to match somebody with somebody The solution for making, continues, in water-bath stirring, to stir 10-30min, then, takes out above-mentioned solution and is cooled down in atmosphere, treats After forming solid flocculence, filtered, solid is dried after filtration, you can obtain CNXLoad diatomite composite material.
2. according to the CN described in claim 1XThe preparation method of load diatomite composite material, it is characterised in that tripolycyanamide The bulking value ratio of quality and diatomaceous quality and dust technology is 1g:1g:10ml.
3. according to the CN described in claim 1XThe preparation method of load diatomite composite material, it is characterised in that the CN for obtainingX The further heat treatment calcining of load diatomite composite material, heat treatment condition is that under air conditionses, heat treatment temperature is 150- 550 DEG C, the time 1-3 hour of heat treatment.
4. the preparation method of diatomite composite material is loaded according to the CNX described in claim 3, it is characterised in that heat treatment temperature Spend for 150-250 DEG C.
5. according to the CN described in claim 3XThe preparation method of load diatomite composite material, it is characterised in that heat treatment time For 2 hours.
6. the CN for preparing according to the method described in any one of claim 1-5XLoad diatomite composite material.
7. the CN for preparing according to the method described in any one of claim 1-5XLoad diatomite composite material, its feature exists In CNXIt is 1-5 with diatomaceous mass ratio:1.
8. the CN for preparing according to the method described in any one of claim 1-5XThe application of load diatomite composite material, its It is characterised by, as adsorbent, for adsorbing congo red.
9. according to the application of claim 8, it is characterised in that by CNXLoad diatomite composite material is added to containing Congo red dye In the waste water of material, mix and stir, make CNXLoad diatomite composite material fully adsorbs Congo red, is then separated by filtration, and removes It is adsorbed with the CN of Congo redXLoad diatomite composite material.
10. according to the application of claim 9, it is characterised in that the initial concentration of Congo red waste water solution is 2000mg/L, often The adsorbent amount added in 50mL Congo red solution is 0.1-0.5g;Carry out concussion absorption:30-50 DEG C of adsorption temp, concussion Adsorption time is 1-5min, and pH value is 6-7.
CN201710011256.6A 2017-01-06 2017-01-06 CNXPreparation of modified diatomite and method for adsorbing Congo red wastewater by using modified diatomite Expired - Fee Related CN106669596B (en)

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Cited By (6)

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CN109107523A (en) * 2018-08-01 2019-01-01 中南林业科技大学 Ultra-thin graphite-phase C3N4/ calcite nanosheet composite material and its preparation method and application
CN109499553A (en) * 2018-12-21 2019-03-22 徐荣霞 A kind of dyeing and printing sewage processing porous spheroidal adsorbent and preparation method thereof
CN110496593A (en) * 2018-05-18 2019-11-26 南京理工大学 Lamellar graphite phase carbon nitride/montmorillonite composite material and its preparation method and application
CN112756008A (en) * 2021-01-13 2021-05-07 合肥工业大学 Iron-doped carbon nitride diatomite composite material and preparation method and application thereof
CN113529491A (en) * 2021-07-02 2021-10-22 武汉梓强生态科技有限公司 Modified diatomite adsorption wallpaper and preparation method thereof
CN115318238A (en) * 2022-08-11 2022-11-11 天津大学 Adsorbent for adsorbing Congo red dye in water and preparation method and application thereof

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CN110496593A (en) * 2018-05-18 2019-11-26 南京理工大学 Lamellar graphite phase carbon nitride/montmorillonite composite material and its preparation method and application
CN109107523A (en) * 2018-08-01 2019-01-01 中南林业科技大学 Ultra-thin graphite-phase C3N4/ calcite nanosheet composite material and its preparation method and application
CN109107523B (en) * 2018-08-01 2021-04-20 中南林业科技大学 Ultra-thin graphite phase C3N4Calcite nanosheet composite material and preparation method and application thereof
CN109499553A (en) * 2018-12-21 2019-03-22 徐荣霞 A kind of dyeing and printing sewage processing porous spheroidal adsorbent and preparation method thereof
CN112756008A (en) * 2021-01-13 2021-05-07 合肥工业大学 Iron-doped carbon nitride diatomite composite material and preparation method and application thereof
CN113529491A (en) * 2021-07-02 2021-10-22 武汉梓强生态科技有限公司 Modified diatomite adsorption wallpaper and preparation method thereof
CN115318238A (en) * 2022-08-11 2022-11-11 天津大学 Adsorbent for adsorbing Congo red dye in water and preparation method and application thereof
CN115318238B (en) * 2022-08-11 2024-01-30 天津大学 Adsorbent for adsorbing Congo red dye in water and preparation method and application thereof

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