CN109126713A - A method of there is photo-catalysis function decolorising agent using the preparation of pulp thickening object - Google Patents
A method of there is photo-catalysis function decolorising agent using the preparation of pulp thickening object Download PDFInfo
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Abstract
The present invention discloses a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent, the following steps are included: (1) adds sulfonated coal into high concentration aqueous's ink jet printing waste liquid, it is stirred to react, extractable matter in waste water is set just to be condensed into insoluble tiny solid particle, and the amine (ammonia) in fixed waste water；(2) high-speed stirred ultrasonication simultaneously heats simultaneously, is then slowly stirred, and forms bulky grain solid extract, stops stirring；(3) it is higher than the above 0-20 DEG C of holding ultrasonication of softening point of water-soluble binder to temperature and keeps the temperature, forms the blocky extract of internal void prosperity；(4) it is shunk sufficiently to extract volume, stops ultrasonication, water cooling down is discharged；(5) it takes out extract to be fully cooled, low temperature drying after being crushed；(6) 500 DEG C of charing 1-4h in Muffle furnace under nitrogen protection by the extract after drying are made and contain C3N4Adsorption decolouriser with photo-catalysis function.
Description
Technical field
It is the invention belongs to environmental protection technical field, in particular to a kind of to be urged using the preparation of stamp pulp thickening object with light
Change the method for function decolorising agent.
Background technique
Ink is made of pigment, binder, filler, additional material etc., can be divided into oil-based ink and water-based ink.Oiliness oil
Contain a large amount of organic solvent in ink, it is seriously polluted, gradually it is eliminated.Water-based ink mainly by water-soluble resin, pigment, alcohol,
Amine or ammonia and other additives and water composition.Water-based ink is wide in every field because of its health, environmental protection, safe characteristic
General application.Currently, a large amount of plastic package material uses water-based ink in stamp, printing more and more, in replacement color
When need to clean printing equipment and water-based ink storage tank, produce a certain amount of high concentration aqueous's ink jet printing waste liquid.This kind print
Containing pollutants such as pigment, water soluble acrylic resin's binder, alcohol, amine (ammonia) in flower waste liquid, content of organics is more, coloration
Height, pollution it is extremely serious (coloration: 30,000 times or more, CODCr: 100,000-50 ten thousand mg/L), it is difficult to it handles.
Processing for this kind of waste liquid generallys use the chemical methodes such as Coagulation Method and is pre-processed, i.e., adds into waste liquid
Coagulant makes pollutant agglomerate to form sludge.Typically directly using sheet frame roll filter, belt type dewaterer or centrifugal dehydrator etc. into
The solid-liquid separating methods such as row mechanical dehydration are separated by solid-liquid separation, and water outlet carries out other chemistry or biological treatment to qualified discharge again.
Since pollutant concentration is high in waste liquid, the sludge solid content of formation is up to 5-10%, it is difficult to dehydration, and pass through machinery pressure
The mud cake formed after filter or centrifugal dehydration carries out landfill or burning disposal usually as solid waste, be easy to cause secondary pollution.
In recent years, domestic and foreign scholars to using various wastes prepare decolorising agent and for dye waste water adsorbing and discoloring carry out
A large amount of research.Decolorising agent is made using industrial washing sludge in such as Ta í sL Silva, balances to reactive dye brilliant blue R
Adsorption capacity is up to 36.5 mgg-1；Decolorising agent is made using weaving sludge in Syieluing Wong etc., to active black and methylene
The equilibrium adsorption capacities of base indigo plant are respectively 5 mgg-1With 3.66 mgg-1；Geethakarthi A etc. utilizes leather-making mud system
Decolorising agent is obtained, it is measured and 39.37mgg is reached to the equilibrium adsorption capacities of REACTIVE RED 31-1；Li Wenhong etc. is dirty using papermaking
Clay decolorising agent, to the equilibrium adsorption capacities of Reactive Red 24 up to 15.68 mgg-1.Decolorising agent is prepared with trade waste,
It not only prevents secondary pollution again and can be realized the resource utilization of solid waste, there is good environmental benefit and social benefit.But
Be sludge base decolorising agent the generally existing dosage of adsorption effect it is big, the low problem of the adsorption equilibrium adsorption capacity to dyestuff.
Containing a large amount of organic matter available resources such as water-based acrylic resin binder in water-based ink sludge, as can will
It is prepared into decolorising agent and is applied to decoloring dye waste water, and the secondary use of sludge may be implemented.A kind of patent of invention " high concentration
The method that black printed waste liquor contamination object is extracted and utilized " (patent No. CN2016109043675) summary of the invention is " by high concentration
The acidification of black water ink jet printing waste liquid, stirring make pollutant agglomerate to form paste sludge；Add 5-10g/L's into sludge
Sludge is heated to 50-90 DEG C of dehydration while stirring after mixing evenly by 100-500 mesh calcium miberal powder, is made sludge curing at bulk, is taken off
Chinese effluent；Take out sludge hot squeeze to moisture percentage in sewage sludge it is dry lower than after 40%；Sludge isolation air after drying is heated to
400-700 DEG C of heat preservation 1-4h；Sludge is cooled to 50 DEG C or less and is broken into graininess, the mist that sprinkling mass concentration is 0.1-0.2%
It is uniformly mixed after shape wetting agent solution；Mud granule is added in cationic dyeing waste water by 2-10g/L waste water dosage,
Aeration stirring 10-120min, precipitating or filtering removal mud granule, decolourize discharge of wastewater；Mud granule recycles 400-700 DEG C of heat
Regeneration is recycled." its be used for cationic dyeing waste water decoloring processing, decolorising agent dosage be 5-10g/L waste water.Such as
Embodiment 1 " 92% concentrated sulfuric acid is slowly added into the high concentration black water ink jet printing waste liquid that COD is 39.2 ten thousand mg/L,
Stirring makes pollutant agglomerate to form sludge；The 200-500 mesh calcium miberal powder of 8g/L is added into sludge, after mixing evenly while stirring
Sludge is heated to 75 DEG C of dehydrations, makes sludge curing at bulk, takes off Chinese effluent；It takes out sludge hot and squeezes to moisture content and be lower than
It is dry after 40%；Sludge isolation air after drying is heated to 500 DEG C of heat preservation 2h；Sludge is cooled to 50 DEG C or less to be broken into
Graininess, sprinkling mass concentration are uniformly mixed after 0.1% misty wetting agent solution；Mud granule is pressed into 5g/L waste water dosage
It being added in cationic yellow dyes dyeing waste-water, aeration stirring 100min, precipitating removal mud granule, decolourize discharge of wastewater,
Cationic yellow dyes dyeing waste-water decolorizing rate reaches 99.5% or more." its decolorising agent dosage be 5g/L waste water, hence it is evident that exist
Adsorption capacity is low, the big defect of decolorising agent dosage.
C3N4It is a kind of typical polymer semiconductor, the CN atom in structure forms the π of height delocalization with sp2 hydridization
Conjugated system.2.7 eV of its forbidden bandwidth, can be absorbed blue violet light of the solar spectrum medium wavelength less than 475, moreover it is possible to effective activation
Molecular oxygen generates superoxide radical for the photocatalytic conversion of organo-functional group and the photocatalytic degradation of organic pollutant.·
If can make that dye can be improved using absorption and photocatalysis comprising the decolorising agent with photo-catalysis function in decolorising agent
Expect waste water decoloring treatment effect, greatly reduce decolorising agent dosage, save the cost improves treatment effect.
Summary of the invention
The invention proposes a kind of methods using the preparation of pulp thickening object with photo-catalysis function decolorising agent, prepare
Contain C3N4Decolorising agent with photo-catalysis function is used for waste water decoloration of cation dyes, can reduce decolorising agent dosage, improves
The utilization rate of decolorising agent.
For achieving the above object, the technical method that the present invention uses are as follows:
A method of there is photo-catalysis function decolorising agent using the preparation of pulp thickening object, which comprises the following steps:
(1) suitable 200-400 mesh powdery sulfonated coal is added in hydrotropism's ink jet printing waste liquid, is stirred to react, is utilized sulfonated coal
The exchangeable ion ionized out inhibits the degree of ionization of the ionogen of water-soluble binder in waste liquid, destroys the steady of binder
It is qualitative, extractable matter in waste liquid is precipitated just into insoluble tiny solid particle, while amine in exchangeable ion and waste liquid
(ammonia) combines, and promotes ion exchange, makes the organic amine (ammonia) in sulfonated coal and the fixed waste liquid of the binder of precipitation；
(2) high-speed stirred waste liquid prevents the tiny solid particles flocculate generated and waste liquid is kept to be uniformly mixed, and adds into waste liquid
5-10g/L is reacted with hydrogen ion in waste liquid generates small CO2The chemical agent of bubble sticks bubble tiny micro- in waste liquid
Grain forms gas, liquid, solid three-phase contact interface between fine particles, Gu reducing solid-contact interface, prevents the flocculation of solia particle
Increase and subsequent cure is excessively closely knit, pH is controlled after reaction and is lower than 9；
(3) slow slow down stirs, is simultaneously heated to softening point of the temperature higher than water-soluble binder or more simultaneously with ultrasonication
0-20 DEG C, cohere tiny solid particle mutually together with the sulfonated coal of fixed organic amine, formed internal package microbubble and
The bulky grain extract of water stops stirring；
(4) keep ultrasonication and keeping the temperature, using binder macromolecular chain roll up and intermolecular force mentions bulky grain
Object is taken sufficiently to cohere, volume is constantly shunk, until forming the extract of internal void prosperity, while utilizing ultrasound in insulating process
Wave and heat effect keep hole between extract internal particle uniform by molecular chain movement, keep extract structure uniform；
(5) it is shunk sufficiently to extract volume, stops ultrasonication, water is discharged, extract surface fast cooling is cooling, make
The quick-hardening of extract surface reduces extract surface viscosity；
(6) blocky extract is taken out after being fully cooled, and extract is lower than to the softening point of water-soluble binder after being crushed in temperature
Dry or natural drying below temperature；
(7) 500 DEG C of carbonization-activation 1-4h in Muffle furnace under nitrogen protection by the extract after drying are made and contain C3N4Have
The decolorising agent of photo-catalysis function.
The utility model has the advantages that
A. high concentration aqueous's ink jet printing waste liquid extracts pollutant process through this method, and waste liquid percent of decolourization is up to 99.8% or more,
For organic pollutant recovery rate up to 95% or more, ammonia nitrogen removal frank reaches 85% or more, is greatly lowered waste liquor contamination load, convenient for useless
Water subsequent processing.
B. the ionization of the hydrogen ion inhibition water soluble polymer binder ionogen ionized out with sulfonated coal, and with
Acrylic resin binder reacts generation-COOH group, advantageously forms internal hydrogen bond, sufficiently coheres conducive to extract particles,
Volume contraction, and deviate from internal moisture, the excessive hydrogen ion of appropriateness can form-SO3 -[R3NH]+And-COO-[R3NH]+, promote
Into ion exchange, the fixed rate of N is improved, to improve C in product3N4Content.
C. with small CO2Bubble sticks the tiny solid particle in waste liquid, forms gas, liquid, solid between tiny solid particle
Three-phase contact interface prevents the flocculation increase of solia particle and subsequent cure excessively closely knit Gu solid-contact interface can be reduced,
Conducive to internal small mesoporous quantity is formed, decolorizing effect is improved.
D. temperature is higher than above 0-20 DEG C of softening point, and binder macromolecular chain can be made sufficiently to shrink, transported by strand
It is dynamic to form the new surface of solids and free volume, interior porosity is further increased, improves decolorizing effect, and make sludge curing
Sufficiently.
E. ultrasonic wave effect can make micro-bubble inside extract acutely vanish, and generate shock wave, cause local agitation, promote
Molecular chain movement is violent, is not only conducive to be formed mesoporous but also keep hole between blocky extract internal particle uniform.
F. extract is further taken out after being fully cooled, can prevent from extracting composition deformation under high temperature, destroys hole between internal particle.
G. decolorising agent prepared by the method for the present invention, the C formed by the nitrogen that sulfonated coal is fixed3N4It is uniformly distributed in decolorising agent,
It no longer needs to be easily recycled use by other carriers.
Detailed description of the invention
Fig. 1 is to contain C in the prepared decolorising agent XRD display decolorising agent of 500 DEG C of extract of the present invention charings3N4, Fig. 2 is
The XRD of extract and different temperatures carbide (2h).
Specific embodiment
The present invention is further illustrated below by specific embodiment.
Embodiment 1
(1) suitable 300 mesh powdery sulfonated coal is added in hydrotropism's ink jet printing waste liquid, is stirred to react, is ionized using sulfonated coal
Exchangeable ion out destroys the stability of binder, so that extractable matter is just condensed into insoluble tiny solid micro-
Grain, while amine (ammonia) combines in exchangeable ion and waste liquid, promotes ion exchange, the organic amine (ammonia) in fixed waste liquid；
(2) high-speed stirred (300r/min) waste liquid prevents the tiny solid particles flocculate generated and waste liquid is kept to be uniformly mixed, to
5g/L sodium bicarbonate is added in waste liquid and reacts generation micro-bubble with waste liquid, and bubble is made to stick the tiny solid particle in waste liquid,
Gas, liquid, solid three-phase contact interface is formed between tiny solid particle, the flocculation increase for preventing solia particle and subsequent cure are excessively
It is closely knit；
(3) it persistently stirs (50r/min), be simultaneously heated to temperature simultaneously with 40KHz ultrasonication higher than water-soluble binder
It more than softening point 10 DEG C, coheres tiny solid particle mutually together with the sulfonated coal of fixed organic amine, forms internal package
The bulky grain solid extract of microbubble and water stops stirring；
(4) keep ultrasonication and keeping the temperature, using binder macromolecular chain roll up and intermolecular force consolidates bulky grain
Body extract sufficiently coheres, and volume is constantly shunk, until forming the blocky extract of internal void prosperity, while in insulating process
Keep hole between blocky extract internal particle uniform by molecular chain movement using ultrasonic wave and heat effect, keeps extract structure
Uniformly；
(5) it is shunk sufficiently to blocky extract volume, stops ultrasonication, water is discharged, by the blocky fast prompt drop in extract surface
Temperature is cooling, makes the quick-hardening of extract surface, reduces extract surface viscosity；
(6) it takes out blocky extract to be fully cooled, extract is lower than to the softening point temperature of water-soluble binder after being crushed in temperature
20 DEG C of degree or less is dry；
(7) decolorising agent is made in 500 DEG C of charing 2h in Muffle furnace under nitrogen protection by the extract after drying.
Embodiment 2
(1) suitable 200-300 mesh powdery sulfonated coal is added in hydrotropism's ink jet printing waste liquid, is stirred to react, is utilized sulfonated coal
The exchangeable ion ionized out inhibits the degree of ionization of the ionogen of water-soluble binder in waste liquid, destroys the steady of binder
It is qualitative, so that extractable matter in waste liquid is just condensed into insoluble tiny solid particle, while amine in exchangeable ion and waste liquid
(ammonia) combines, and promotes ion exchange, the organic amine (ammonia) in fixed waste liquid；
(2) high-speed stirred (300r/min) waste liquid prevents the tiny solid particles flocculate generated and waste liquid is kept to be uniformly mixed, to
The potassium carbonate of 10g/L is added in waste liquid and waste liquid reacts and generates micro-bubble, and bubble is made to stick the tiny solid particle in waste liquid,
Gas, liquid, solid three-phase contact interface is formed between tiny solid particle, Gu reducing solid-contact interface, prevents the wadding of solia particle
Solidifying increase and subsequent cure are excessively closely knit；
(3) it persistently stirs (60r/min), be simultaneously heated to temperature simultaneously with 40KHz ultrasonication higher than water-soluble binder
It more than softening point 5 DEG C, coheres tiny solid particle mutually together with the sulfonated coal of fixed organic amine, it is micro- to form internal package
The bulky grain solid extract of bubble and water stops stirring；
(4) keep ultrasonication and keeping the temperature, using binder macromolecular chain roll up and intermolecular force consolidates bulky grain
Body extract sufficiently coheres, and volume is constantly shunk, until forming the blocky extract of internal void prosperity, while in insulating process
Keep hole between blocky extract internal particle uniform by molecular chain movement using ultrasonic wave and heat effect, keeps extract structure
Uniformly；
(5) it is shunk sufficiently to blocky extract volume, stops ultrasonication, water is discharged, by the blocky fast prompt drop in extract surface
Temperature is cooling, makes the quick-hardening of extract surface, reduces extract surface viscosity；
(6) it takes out blocky extract to be fully cooled, extract is lower than to the softening point temperature of water-soluble binder after being crushed in temperature
20 DEG C of degree or less is dry；
(7) decolorising agent is made in 500 DEG C of charing 3h in Muffle furnace under nitrogen protection by the extract after drying.
Embodiment 3
(1) suitable 300-400 mesh powdery sulfonated coal is added in hydrotropism's ink jet printing waste liquid, is stirred to react, is utilized sulfonated coal
The exchangeable ion ionized out inhibits the degree of ionization of the ionogen of water-soluble binder in waste liquid, destroys the steady of binder
It is qualitative, so that extractable matter in waste liquid is just condensed into insoluble tiny solid particle, while amine in exchangeable ion and waste liquid
(ammonia) combines, and promotes ion exchange, the organic amine (ammonia) in fixed waste liquid；
(2) high-speed stirred (200r/min) waste liquid prevents the tiny solid particles flocculate generated and waste liquid is kept to be uniformly mixed, to
10g/L sodium carbonate is added in waste liquid and reacts generation micro-bubble with waste liquid, and bubble is made to stick the tiny solid particle in waste liquid,
Gas, liquid, solid three-phase contact interface is formed between tiny solid particle, Gu reducing solid-contact interface, prevents the flocculation of solia particle
Increase and subsequent cure is excessively closely knit；
(3) it persistently stirs (60r/min), be simultaneously heated to temperature simultaneously with 40KHz ultrasonication higher than water-soluble binder
It more than softening point 20 DEG C, coheres tiny solid particle mutually together with the sulfonated coal of fixed organic amine, forms internal package
The bulky grain solid extract of microbubble and water stops stirring；
(4) keep ultrasonication and keeping the temperature, using binder macromolecular chain roll up and intermolecular force consolidates bulky grain
Body extract sufficiently coheres, and volume is constantly shunk, until forming the blocky extract of internal void prosperity, while in insulating process
Keep hole between blocky extract internal particle uniform by molecular chain movement using ultrasonic wave and heat effect, keeps extract structure
Uniformly；
(5) it is shunk sufficiently to blocky extract volume, stops ultrasonication, water is discharged, by the blocky fast prompt drop in extract surface
Temperature is cooling, makes the quick-hardening of extract surface, reduces extract surface viscosity；
(6) it takes out blocky extract to be fully cooled, spontaneously dries extract after broken；
(7) decolorising agent is made in 500 DEG C of charing 2.5h in Muffle furnace under nitrogen protection by the extract after drying.
Decolorising agent made from embodiment 1, embodiment 2, embodiment 3 is used for cationic blue X- under sunlight irradiation respectively
The decolorization 6h of GRRL dye solution, is then separated by filtration removal decolorising agent, and it is remaining to survey dye solution by spectrophotometer
Concentration, tests solution decolorizing effect, and result is as shown in the table.
By decolorizing effect in table as it can be seen that prepared decolorising agent is 0.6g/ to the dye of positive ion solution dosage of concentration 300mg/L
When L solution or so, for solution percent of decolourization up to 98% or more, decolorising agent dosage is low, improves the utilization rate of decolorising agent.With other dirts
Mud base decolorising agent is compared, and for the dye solution of same concentrations, reaches identical decolorizing effect, decolorising agent prepared by the present invention is thrown
Dosage is few, that is, can reach good decolorizing effect.It is de- in 400 DEG C and 600 DEG C charing 2h products with the extract referring to embodiment 1
Color effect is compared, and percent of decolourization improves 20% or more.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any those skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its invent
Design is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent, which is characterized in that including following step
It is rapid:
(1) suitable 200-400 mesh powdery sulfonated coal is added in hydrotropism's ink jet printing waste liquid, is stirred to react, is utilized sulfonated coal
The exchangeable ion ionized out inhibits the ionization of the ionogen of water-soluble binder in waste liquid, destroys the stabilization of binder
Property, extractable matter is precipitated just and forms fine particles, while organic amine (ammonia) is tied in exchangeable ion and waste liquid
It closes, promotes ion exchange, make the organic amine (ammonia) in sulfonated coal and the fixed waste liquid of the binder of precipitation；
(2) quickly stirring waste liquid prevents the fine particles generated from flocculating and waste liquid is kept to be uniformly mixed, and 5- is added into waste liquid
10g/L is reacted with waste liquid generates small CO2The chemical agent of bubble makes bubble stick the fine particles in waste liquid, tiny micro-
Intergranular forms gas, liquid, solid three-phase contact interface, solid to reduce solid-contact interface, prevents the flocculation increase of solia particle and subsequent
Solidification is excessively closely knit, and pH is controlled after reaction and is lower than 9；
(3) slow slow down stirs, is simultaneously heated to softening point of the temperature higher than water-soluble binder or more simultaneously with ultrasonication
It 0-20 DEG C, coheres fine particles mutually with sulfonated coal, forms the bulky grain extract of internal package microbubble and water, stop
Only stir；
(4) ultrasonication and held for some time are kept, using binder macromolecular chain roll up and intermolecular force makes
Bulky grain extract sufficiently coheres, and volume is constantly shunk, until forming the extract of internal void prosperity, while in insulating process
Keep hole between extract internal particle uniform by molecular chain movement using ultrasonic wave and heat effect, keeps extract structure equal
It is even；
(5) it is shunk sufficiently to extract volume, stops ultrasonication, water is discharged, extract surface fast cooling is cooling, make
The quick-hardening of extract surface reduces extract surface viscosity；
(6) extract is taken out after being fully cooled, and extract is lower than to the softening point temperature of water-soluble binder after being crushed in temperature
Dry below or natural drying；
(7) 500 DEG C of carbonization-activation 1-4h in Muffle furnace under nitrogen protection by the extract after drying are made and contain C3N4Have
The decolorising agent of photo-catalysis function.
2. a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent according to claim 1,
It is characterized in that, the sulfonated coal in the step (1) is Hydrogen sulfonated coal, need to be handled in advance with acid if sodium form sulfonated coal.
3. a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent according to claim 1,
It is characterized in that, the chemical agent in the step (2) is or mixtures thereof water soluble carbonate hydrogen salt or one kind of carbonate.
4. a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent according to claim 1,
It is characterized in that, the quick speed of agitator in the step (2) is not less than 200r/min.
5. a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent according to claim 1,
It is characterized in that, the slow deceleration speed of agitator in the step (3) is not higher than 60r/min.
6. a kind of side using the preparation of stamp pulp thickening object with photo-catalysis function decolorising agent according to claim 1
Method, which is characterized in that ultrasonic frequency is greater than 20KHz in the step (3), (4).
7. a kind of method using the preparation of pulp thickening object with photo-catalysis function decolorising agent according to claim 1,
It is characterized in that, soaking time is 10-60min in the step (4).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111715175A (en) * | 2019-03-21 | 2020-09-29 | 中国科学院上海硅酸盐研究所 | Carbonate modified carbon nitride, preparation method thereof and application thereof in low-concentration ammonia nitrogen wastewater treatment |
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| CN105621739A (en) * | 2016-01-19 | 2016-06-01 | 青岛大学 | Printing waste liquid synchronous decolorization and nitrogen recovery method and device |
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| CN105084703A (en) * | 2014-05-05 | 2015-11-25 | 青岛大学 | Microwave irradiation dehydration method for wax-recovered sludge in wax printing waste water |
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| CN111715175B (en) * | 2019-03-21 | 2021-06-15 | 中国科学院上海硅酸盐研究所 | Carbonate modified carbon nitride, preparation method thereof and application thereof in low-concentration ammonia nitrogen wastewater treatment |
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