CN106334535A - Preparation method of adsorbing material for removing Congo red in dye wastewater - Google Patents
Preparation method of adsorbing material for removing Congo red in dye wastewater Download PDFInfo
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- CN106334535A CN106334535A CN201610945065.2A CN201610945065A CN106334535A CN 106334535 A CN106334535 A CN 106334535A CN 201610945065 A CN201610945065 A CN 201610945065A CN 106334535 A CN106334535 A CN 106334535A
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- congo red
- paulownia
- attapulgite
- verniciae fordii
- oleum verniciae
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a preparation method of an adsorbing material for removing Congo red in dye wastewater and belongs to the technical field of sewage treatment. The preparation method comprises the steps that firstly, China wood oil is extracted from China wood seeds and is mixed with attapulgite to obtain turbid mixed liquid, a certain proportion of ferrous nitrate and nickel nitrate mixed liquid is prepared, the turbid mixed liquid is added, a sodium hydroxide solution is added dropwise, particulate matter is obtained through precipitation, filtration, drying and high-temperature calcination and is soaked with domestic kitchen wastewater, filtration is performed, fermentation is performed under anaerobic condition, then the particulate matter is constantly subjected to drip washing by using China wood oil to make mould grow, air is isolated by using nitrogen under ultraviolet light to perform high temperature activation, and then the adsorbing material for removing the Congo red in dye wastewater is obtained. The invention provides a method for treating a dye Congo red. The operation is simple, the cost is low, the prepared adsorbent has the advantages of being good in absorption property, obviously reducing the Congo red concentration and the like, and accordingly comprehensive resource utilization, low cost and high-efficiency dye wastewater purification are achieved.
Description
Technical field
The invention discloses a kind of preparation method for removing Congo red adsorbing material in waste water from dyestuff, belong at sewage
Reason technical field.
Background technology
Dyestuff plays a very important role in daily life, has greatly weaving, papermaking etc. are industrial
Application, just because of its presence, make our life become bright and colourful.At present, China's various dyestuff yield has reached 900,000
Ton, waste water from dyestuff has become one of environment major polluting sources.Contain substantial amounts of Organic substance and salt in its waste water, there is codcr
Height, color and luster is deep, the features such as Acidity of Aikalinity is strong, the always difficult problem in wastewater treatment.This not only causes great economic loss,
Bring serious pollution to environment, in numerous fuel, azo dye is the organic conjunction of one kind most widely used, that quantity is most
Become fuel, wherein Congo red is a kind of anionic dye of typical diphenyl amine azo direct, it is producing and is using process
Middle turnover rate is high, easily enters water body, has destruction to ecological environment.Congo red waste water has that change of water quality is big, colourity
The features such as high with cod, it is one of common pollutant in waste water from dyestuff, side effect is many, complicated component is it is difficult to degradation treatment.
Existing treatment technology such as flocculant, the method such as decolorising agent, oxidoreduction, absorption, brucite adsorbing material.Typically
Flocculant, decolorising agent the Congo red in waste water cannot be removed, reasonable adsorbent reactivation is difficult, oxidant
The drawbacks of amount ratio is larger, and absorption method be because introducing new pollutant, energy consumption is relatively low and concentration and separation can have from waste water
Organic pollutants, thus receive significant attention.White rot fungi (white rot fungi) is the saprophytic filamentous fungis of a class, due to
Its secretion extracellular lignin-degrading enzymes have non-specificity and without substrate for induction special performance so that it is to many structures
Difference, high toxicity, macromolecule hardly degraded organic substance, such as azo dyes have degradation capability.But there is intensity relatively in white rot fungi
Low, mass-transfer performance is poor, affects cytoactive, and regeneration is difficult, easily by biological decomposition the problems such as.Attapulgite used in the present invention
Land reform, compared with other adsorbing materials, has significantly single-minded adsorptivity, and adsorbance is big, and clearance is high, is prepared into simultaneously
This low it is achieved that the comprehensive utilization of resource.
Content of the invention
The invention mainly solves the technical problem of: it is difficult to remove for ease of solubility congo red in dyeing waste water, and
It is low to there is adsorbance in tradition absorption Congo red material, easy saturation, regeneration this drawback difficult, there is provided a kind of using natural organic
Thing modification mesoporous adsorption material pore structure, fermentable solidifies mesoporous adsorption material specific surface area, loads the corresponding and the Congo
The adsorbing material preparation method of reddish tint molten organic group.The present invention, with ferrous nitrate and nickel nitrate as base material, adds appropriate paulownia
The modified attapulgite of oil, is precipitated in alkaline environment, is obtained mesoporous material by high-temperature calcination；With mesoporous material it is again
Supporting body, kitchen sanitary sewage is microbial source, and Oleum Verniciae fordii is microorganism organic nutrient solution for cultivating, and lasting anaerobic fermentation is mouldy, until mould
Bacterium penetrates lower inactivation in sunlight, and solidification has the Organic substance of corresponding function group on its surface, reaches in removal dyeing waste water just
The purpose of arnotto；The present invention, compared with other adsorbing materials, has significantly single-minded adsorptivity, and adsorbance is big, and clearance is high,
More than 10 times its clearances of circulation absorption are not decreased obviously, simultaneously preparation cost low it is achieved that the comprehensive utilization of resource.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) the ripe paulownia seed of selected 1～2kg, being placed in is exposed to the sun under the sun splits to paulownia seed, subsequently shells, sort out paulownia seed core, will
It cleans dry in the sun afterwards is 2～5% to paulownia seed core water content, and the paulownia processing seed core is put into crusher for crushing, and excessively 20～
25 mesh sieves, obtain paulownia seed powder, are placed in oil press, extracted oil at 130～160 DEG C, subsequently fuel-displaced, obtain rough paulownia
Oil, through filtering, removes the impurity in Oleum Verniciae fordii, obtains filtrate, and by the filtrate of gained under the conditions of temperature is 30～40 DEG C, standing is heavy
Form sediment 5～10 days, take the supernatant, obtain final product refined Oleum Verniciae fordii；
(2) 1:10 in mass ratio, attapulgite is soaked in above-mentioned gained and refines 12～24h in Oleum Verniciae fordii, treat attapulgite saturation
Afterwards, filter, obtain saturation Oleum Verniciae fordii attapulgite, saturation Oleum Verniciae fordii attapulgite is mixed with deionized water 1:8 in mass ratio, is placed in super
In sonication instrument, 15～30min is stirred with 300～600r/min rotating speed, then move into ultrasonic in 50～80 DEG C of constant temperature oscillation beds
Vibration 25～45min, must mix turbid liquid；
(3) measure 300～400ml mass fraction 35%～55% ferrous nitrate solution and 300～400ml mass fraction be 35%～
55% nickel nitrate solution mixing, obtains mixed solution, and the mixing turbid liquid volume ratio pressing mixed solution after mixing with above-mentioned preparation is 3:7,
Mixed liquor is uniformly mixing to obtain with 300～500r/min；
(4) continuous Deca 0.5～1.0mol/l sodium hydroxide solution in the mixed liquor of above-mentioned preparation, and with 400～700r/
Min stirring, until precipitation completely, filters, is collected filter cake, and in an oven, temperature is carried out drying 2～3h for 105～110 DEG C, obtains
To dried object, move it in calcining furnace, after calcining 2～3h under nitrogen protective condition at 800～900 DEG C, pulverize and cross 120
～180 mesh sieves, obtain the particulate matter that sieves；
(5) by above-mentioned gained sieve particulate matter be soaked in anaerobic fermentation 12 in the anaerobic jar being placed in sealing in sanitary sewage～
24h, period, adds 10～15ml rubbish from cooking every 1～2h, is further continued for anaerobic fermentation 2～3 days, after the completion of fermentation, filters,
Filtrate, dry, and in the case of ventilation, take mass fraction to be 3% ~ 5% malic acid solution in 20 ~ 25 DEG C of temperature, relatively
Humidity every 2～3h drip washing once, observes surface particles fungus growth under 80%～90% environment；
(6) treat that above-mentioned surface particles fungus growth, to 5～10mm, is put the 30～60min that is exposed to the sun under strong sunlight and moved into 180 again
In～200 DEG C of baking ovens, continuous baking 1～2h under nitrogen protective condition, obtain final product a kind of adsorbing material of absorption Congo red.
The application process of the present invention: take 1～3l dye house effluents, measuring its methylene blue count is 300～500mg/l,
The adsorbing material removing dyeing waste water Methylene Blue that 1～3g present invention is obtained is added under 400～600r/min stirring, then
Move into vibration bed vibration 5～10min, static 15～30min, measuring its waste water methylene content is below 0.5mg/l, removes
Rate reaches more than 99%；10 experiments of circulation absorption, its clearance, still more than 99%, is iteratively repeated absorption until absorption reaches
To saturation, dried for after 18% salt acid elution with 0.5m sodium hydroxide and mass fraction respectively, dry in 150～180 ° of c baking ovens
Roasting 2～3h, you can regeneration, to dyeing waste water Methylene Blue clearance up to more than 98% after regeneration.
The invention has the beneficial effects as follows:
(1) gained of the present invention remove Congo red in waste water from dyestuff adsorbing material simple to operate, treatment effect is substantially and stability
Good, thoroughly, percent of decolourization is up to more than 98% for Congo red decolored degradation；
(2) in gained removal waste water from dyestuff of the present invention, the adsorbing material of Congo red can be degraded by environmental microorganism after discarding, will not
Cause secondary pollution.
Specific embodiment
The ripe paulownia seed of selected 1～2kg, being placed in is exposed to the sun under the sun splits to paulownia seed, subsequently shells, sort out paulownia seed core,
After being cleaned, dry in the sun is 2～5% to paulownia seed core water content, and the paulownia processing seed core is put into crusher for crushing, and crosses 20
～25 mesh sieves, obtain paulownia seed powder, are placed in oil press, extracted oil at 130～160 DEG C, subsequently fuel-displaced, obtain rough paulownia
Oil, through filtering, removes the impurity in Oleum Verniciae fordii, obtains filtrate, and by the filtrate of gained under the conditions of temperature is 30～40 DEG C, standing is heavy
Form sediment 5～10 days, take the supernatant, obtain final product refined Oleum Verniciae fordii；1:10 in mass ratio, attapulgite is soaked in above-mentioned gained and refines paulownia
Oil in 12～24h, after attapulgite saturation, filter, obtain saturation Oleum Verniciae fordii attapulgite, by saturation Oleum Verniciae fordii attapulgite with go from
Sub- water 1:8 in mass ratio mixes, and is placed in supersonic oscillations instrument and stirs 15～30min with 300～600r/min rotating speed, then move
Enter sonic oscillation 25～45min in 50～80 DEG C of constant temperature oscillation beds, turbid liquid must be mixed；Measure 300～400ml mass fraction 35%
～55% ferrous nitrate solution is mixed for 35%～55% nickel nitrate solution with 300～400ml mass fraction, obtains mixed solution, mixes
The mixing turbid liquid volume ratio pressing mixed solution after conjunction with above-mentioned preparation is 3:7, is uniformly mixing to obtain mixing with 300～500r/min
Liquid；Continuous Deca 0.5～1.0mol/l sodium hydroxide solution in the mixed liquor of above-mentioned preparation, and stirred with 400～700r/min
Mix until precipitation completely, filters, collect filter cake, and in an oven, temperature carries out drying 2～3h for 105～110 DEG C, is done
Dry thing, moves it in calcining furnace, under nitrogen protective condition at 800～900 DEG C calcining 2～3h after, pulverize and cross 120～
180 mesh sieves, obtain the particulate matter that sieves；By above-mentioned gained sieve particulate matter be soaked in be placed in sanitary sewage seal anaerobic jar
Interior anaerobic fermentation 12～24h, period, adds 10～15ml rubbish from cooking every 1～2h, is further continued for anaerobic fermentation 2～3 days, send out
After the completion of ferment, filter, obtain filtrate, dry, and in the case of ventilation, take mass fraction to be 3% ~ 5% malic acid solution in temperature
20 ~ 25 DEG C of degree, relative humidity every 2～3h drip washing once, observes surface particles fungus growth under 80%～90% environment；
Treat above-mentioned surface particles fungus growth to 5～10mm, put the 30～60min that is exposed to the sun under strong sunlight and move into 180～200 DEG C again
In baking oven, continuous baking 1～2h under nitrogen protective condition, obtain final product a kind of adsorbing material of absorption Congo red.
Example 1
The ripe paulownia seed of selected 1kg, being placed in is exposed to the sun under the sun splits to paulownia seed, subsequently shells, sort out paulownia seed core, is cleaned
Dry in the sun is 2% to paulownia seed core water content afterwards, and the paulownia processing seed core is put into crusher for crushing, and crosses 20 mesh sieves, obtains paulownia seed
Powder, is placed in oil press, is extracted oil at 130 DEG C, subsequently fuel-displaced, obtains rough Oleum Verniciae fordii, through filtering, removes in Oleum Verniciae fordii
Impurity, obtain filtrate, and by the filtrate of gained in temperature be 30 DEG C under the conditions of, staticly settle 5 days, take the supernatant, obtain final product essence
Oleum Verniciae fordii processed；1:10 in mass ratio, attapulgite is soaked in above-mentioned gained and refines 12h in Oleum Verniciae fordii, after attapulgite saturation, mistake
Filter, obtains saturation Oleum Verniciae fordii attapulgite, saturation Oleum Verniciae fordii attapulgite is mixed with deionized water 1:8 in mass ratio, is placed in ultrasound wave
In shaker, 15min is stirred with 300r/min rotating speed, then move into sonic oscillation 25min in 50 DEG C of constant temperature oscillation beds, must mix turbid
Liquid；Measure 300ml mass fraction 35% ferrous nitrate solution to mix for 35% nickel nitrate solution with 300ml mass fraction, obtain mixing
Solution, the mixing turbid liquid volume ratio pressing mixed solution after mixing with above-mentioned preparation is 3:7, is uniformly mixing to obtain mixed with 300r/min
Close liquid；Continuous Deca 0.5mol/l sodium hydroxide solution in the mixed liquor of above-mentioned preparation, and with 400r/min stirring until sinking
Form sediment completely, filter, collect filter cake, and in an oven, temperature carries out drying 2h for 105 DEG C, obtains dried object, moves it into calcining
In stove, after calcining 2h under nitrogen protective condition at 800 DEG C, pulverize and cross 120 mesh sieves, obtain the particulate matter that sieves；By above-mentioned institute
The particulate matter that must sieve is soaked in anaerobic fermentation 12h in the anaerobic jar being placed in sealing in sanitary sewage, period, adds every 1h
10ml rubbish from cooking, is further continued for anaerobic fermentation 2 days, after the completion of fermentation, filters, obtains filtrate, dry, and the situation in ventilation
Under, take mass fraction to be 3% malic acid solution in 20 DEG C of temperature, relative humidity be under 80% environment every 2h drip washing once, observe
Surface particles fungus growth；Treat above-mentioned surface particles fungus growth to 5mm, put the 30min that is exposed to the sun under strong sunlight and move again
Enter in 180 DEG C of baking ovens, continuous baking 1h under nitrogen protective condition, obtain final product a kind of adsorbing material of absorption Congo red.
Take 1l dye house effluents, measure its methylene blue count be 300mg/l, 400r/min stirring under add 1g this
The adsorbing material of bright prepared removal dyeing waste water Methylene Blue, then move into vibration bed vibration 5min, static 15min, measure
Its waste water methylene content is 0.3mg/l, and clearance reaches 99.9%；10 experiments of circulation absorption, its clearance still exists
More than 99%, it is iteratively repeated absorption until absorption reaches saturation, use 0.5m sodium hydroxide and mass fraction to be 18% hydrochloric acid respectively
Dry after washing, in 150 ° of c baking ovens toast 2h, you can regeneration, after regeneration to dyeing waste water Methylene Blue clearance up to
More than 98%.
Example 2
The ripe paulownia seed of selected 1.5kg, being placed in is exposed to the sun under the sun splits to paulownia seed, subsequently shells, sort out paulownia seed core, is washed
Only after, dry in the sun is 3% to paulownia seed core water content, and the paulownia processing seed core is put into crusher for crushing, and crosses 23 mesh sieves, obtains paulownia
Seed powder, is placed in oil press, is extracted oil at 140 DEG C, subsequently fuel-displaced, obtains rough Oleum Verniciae fordii, through filtering, removes Oleum Verniciae fordii
In impurity, obtain filtrate, and by the filtrate of gained in temperature be 35 DEG C under the conditions of, staticly settle 7 days, take the supernatant, obtain final product
Refined Oleum Verniciae fordii；1:10 in mass ratio, attapulgite is soaked in above-mentioned gained and refines 16h in Oleum Verniciae fordii, after attapulgite saturation,
Filter, obtain saturation Oleum Verniciae fordii attapulgite, saturation Oleum Verniciae fordii attapulgite is mixed with deionized water 1:8 in mass ratio, is placed in ultrasonic
In ripple shaker, 20min is stirred with 400r/min rotating speed, then move into sonic oscillation 30min in 70 DEG C of constant temperature oscillation beds, obtain mixing
Turbid liquid；Measure 350ml mass fraction 45% ferrous nitrate solution to mix for 45% nickel nitrate solution with 350ml mass fraction, obtain mixed
Close solution, the mixing turbid liquid volume ratio pressing mixed solution after mixing with above-mentioned preparation is 3:7, is uniformly mixing to obtain with 400r/min
Mixed liquor；Continuous Deca 0.7mol/l sodium hydroxide solution in the mixed liquor of above-mentioned preparation, and with 650r/min stirring until
Precipitation completely, filters, and collects filter cake, and in an oven, temperature carries out drying 2.5h for 106 DEG C, obtains dried object, moves it into
In calcining furnace, after calcining 2.5h under nitrogen protective condition at 850 DEG C, pulverize and cross 160 mesh sieves, obtain the particulate matter that sieves；Will
Above-mentioned gained sieve particulate matter be soaked in be placed in sanitary sewage seal anaerobic jar in anaerobic fermentation 14h, period, every
1.5h adds 13ml rubbish from cooking, is further continued for anaerobic fermentation 2.5 days, after the completion of fermentation, filters, obtains filtrate, dry, and logical
In the case of wind, mass fraction is taken to be 4% malic acid solution in 23 DEG C of temperature, relative humidity is to drench every 2.5h under 85% environment
Wash once, observe surface particles fungus growth；Treat above-mentioned surface particles fungus growth to 6mm, put sudden and violent under strong sunlight
Shine 50min and move in 190 DEG C of baking ovens again, continuous baking 1.5h under nitrogen protective condition, obtain final product a kind of suction of absorption Congo red
Enclosure material.
Take 2l dye house effluents, measure its methylene blue count be 400mg/l, 500r/min stirring under add 2g this
The adsorbing material of bright prepared removal dyeing waste water Methylene Blue, then move into vibration bed vibration 8min, static 17min, measure
Its waste water methylene content is below 0.2mg/l, and clearance reaches 99.95%；10 experiments of circulation absorption, its clearance is still
So more than 99%, it is iteratively repeated absorption until absorption reaches saturation, use 0.5m sodium hydroxide and mass fraction to be 18% respectively
Dry after salt acid elution, 160 ° of c baking ovens toast 2.5h, you can regeneration, after regeneration, dyeing waste water Methylene Blue is removed
Rate is up to more than 98%.
Example 3
The ripe paulownia seed of selected 2kg, being placed in is exposed to the sun under the sun splits to paulownia seed, subsequently shells, sort out paulownia seed core, is cleaned
Dry in the sun is 5% to paulownia seed core water content afterwards, and the paulownia processing seed core is put into crusher for crushing, and crosses 25 mesh sieves, obtains paulownia seed
Powder, is placed in oil press, is extracted oil at 160 DEG C, subsequently fuel-displaced, obtains rough Oleum Verniciae fordii, through filtering, removes in Oleum Verniciae fordii
Impurity, obtain filtrate, and by the filtrate of gained in temperature be 40 DEG C under the conditions of, staticly settle 10 days, take the supernatant, obtain final product essence
Oleum Verniciae fordii processed；1:10 in mass ratio, attapulgite is soaked in above-mentioned gained and refines 24h in Oleum Verniciae fordii, after attapulgite saturation, mistake
Filter, obtains saturation Oleum Verniciae fordii attapulgite, saturation Oleum Verniciae fordii attapulgite is mixed with deionized water 1:8 in mass ratio, is placed in ultrasound wave
In shaker, 30min is stirred with 600r/min rotating speed, then move into sonic oscillation 45min in 80 DEG C of constant temperature oscillation beds, must mix turbid
Liquid；Measure 400ml mass fraction 55% ferrous nitrate solution to mix for 55% nickel nitrate solution with 400ml mass fraction, obtain mixing
Solution, the mixing turbid liquid volume ratio pressing mixed solution after mixing with above-mentioned preparation is 3:7, is uniformly mixing to obtain mixed with 500r/min
Close liquid；Continuous Deca 1.0mol/l sodium hydroxide solution in the mixed liquor of above-mentioned preparation, and with 700r/min stirring until sinking
Form sediment completely, filter, collect filter cake, and in an oven, temperature carries out drying 3h for 110 DEG C, obtains dried object, moves it into calcining
In stove, after calcining 3h under nitrogen protective condition at 900 DEG C, pulverize and cross 180 mesh sieves, obtain the particulate matter that sieves；By above-mentioned institute
The particulate matter that must sieve is soaked in anaerobic fermentation 24h in the anaerobic jar being placed in sealing in sanitary sewage, period, adds every 2h
15ml rubbish from cooking, is further continued for anaerobic fermentation 3 days, after the completion of fermentation, filters, obtains filtrate, dry, and the situation in ventilation
Under, take mass fraction to be 5% malic acid solution in 25 DEG C of temperature, relative humidity be under 90% environment every 3h drip washing once, observe
Surface particles fungus growth；Treat above-mentioned surface particles fungus growth to 10mm, put the 60min that is exposed to the sun under strong sunlight and move again
Enter in 200 DEG C of baking ovens, continuous baking 2h under nitrogen protective condition, obtain final product a kind of adsorbing material of absorption Congo red.
Take 3l dye house effluents, measure its methylene blue count be 500mg/l, 600r/min stirring under add 3g this
The adsorbing material of bright prepared removal dyeing waste water Methylene Blue, then move into vibration bed vibration 10min, static 30min, measure
Its waste water methylene content is 0.1mg/l, and clearance reaches more than 99.98%；10 experiments of circulation absorption, its clearance is still
So more than 99%, it is iteratively repeated absorption until absorption reaches saturation, use 0.5m sodium hydroxide and mass fraction to be 18% respectively
Dry after salt acid elution, 180 ° of c baking ovens toast 3h, you can regeneration, to dyeing waste water Methylene Blue clearance after regeneration
Up to more than 98%.
Claims (1)
1. a kind of preparation method for removing Congo red adsorbing material in waste water from dyestuff is it is characterised in that concrete preparation process
For:
(1) the ripe paulownia seed of selected 1～2kg, being placed in is exposed to the sun under the sun splits to paulownia seed, subsequently shells, sort out paulownia seed core, will
It cleans dry in the sun afterwards is 2～5% to paulownia seed core water content, and the paulownia processing seed core is put into crusher for crushing, and excessively 20～
25 mesh sieves, obtain paulownia seed powder, are placed in oil press, extracted oil at 130～160 DEG C, subsequently fuel-displaced, obtain rough paulownia
Oil, through filtering, removes the impurity in Oleum Verniciae fordii, obtains filtrate, and by the filtrate of gained under the conditions of temperature is 30～40 DEG C, standing is heavy
Form sediment 5～10 days, take the supernatant, obtain final product refined Oleum Verniciae fordii；
(2) 1:10 in mass ratio, attapulgite is soaked in above-mentioned gained and refines 12 ~ 24h in Oleum Verniciae fordii, treat attapulgite saturation
Afterwards, filter, obtain saturation Oleum Verniciae fordii attapulgite, saturation Oleum Verniciae fordii attapulgite is mixed with deionized water 1:8 in mass ratio, is placed in super
Stir 15～30min in sonication instrument, then move into sonic oscillation 25～45min in 50～80 DEG C of constant temperature oscillation beds, obtain mixing
Turbid liquid；
(3) measure 300～400ml mass fraction 35% ~ 55% ferrous nitrate solution and 300～400ml mass fraction be 35% ~
55% nickel nitrate solution mixing, obtains mixed solution, and the mixing turbid liquid volume ratio pressing mixed solution after mixing with above-mentioned preparation is 3:7,
Mixed liquor is uniformly mixing to obtain with 300 ~ 500r/min；
(4) continuous Deca 0.5～1.0mol/l sodium hydroxide solution in the mixed liquor of above-mentioned preparation, and with 400 ~ 700r/
Min stirring, until precipitation completely, filters, is collected filter cake, and in an oven, temperature is carried out drying 2～3h for 105～110 DEG C, obtains
To dried object, move it in calcining furnace, after calcining 2～3h under nitrogen protective condition at 800～900 DEG C, pulverize and cross 120
~ 180 mesh sieves, obtain the particulate matter that sieves；
(5) by above-mentioned gained sieve particulate matter be soaked in anaerobic fermentation 12 in the anaerobic jar being placed in sealing in sanitary sewage ~
24h, period, adds 10～15ml rubbish from cooking every 1～2h, is further continued for anaerobic fermentation 2 ~ 3 days, after the completion of fermentation, filters, obtains
Filtrate, dries, and in the case of ventilation, takes mass fraction to be 3% ~ 5% malic acid solution in 20 ~ 25 DEG C of temperature, relatively wet
Spend and every 2～3h drip washing once, observe surface particles fungus growth under 80%～90% environment；
(6) treat that above-mentioned surface particles fungus growth, to 5～10mm, is put the 30～60min that is exposed to the sun under strong sunlight and moved into 180 again
In ~ 200 DEG C of baking ovens, continuous baking 1～2h under nitrogen protective condition, obtain final product a kind of adsorbing material of absorption Congo red.
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| CN109999789A (en) * | 2019-05-20 | 2019-07-12 | 西北师范大学 | A kind of preparation and application of palygorskite/Zn-Mg-Cr ternary metal oxide composite photo-catalyst |
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