CN107628665A - A kind for the treatment of by catalytic oxidation of alkali decrement waste water - Google Patents
A kind for the treatment of by catalytic oxidation of alkali decrement waste water Download PDFInfo
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- CN107628665A CN107628665A CN201710879864.9A CN201710879864A CN107628665A CN 107628665 A CN107628665 A CN 107628665A CN 201710879864 A CN201710879864 A CN 201710879864A CN 107628665 A CN107628665 A CN 107628665A
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- charcoal
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Abstract
The invention discloses a kind for the treatment of by catalytic oxidation of alkali decrement waste water and application.Comprise the following steps：At 50~70 DEG C, charcoal is placed in nitric acid and soaked, and rinsed and no longer change to pH value；By FeSO4·7H2O is dissolved in deionized water, obtains mixed solution after adding absolute ethyl alcohol, charcoal is added into mixed solution, and lasting stirring makes charcoal be sufficiently mixed with solution；Under inert gas shielding, KBH is added dropwise4Solution, reaction is aged after being added dropwise to complete, scrubbed and drying process, it is standby that charcoal load nano zero-valence iron catalyst is made；Charcoal load nano zero-valence iron catalyst is added in alkali decrement waste water, adds Na2S2O8, reacted under normal temperature condition, take out reacted mixed liquor measure CODcr concentration.The method of the present invention is that a kind of technique is simple, oxidation efficiency is high, the alkali decrement waste water treatment by catalytic oxidation of non-secondary pollution.
Description
Technical field
The invention belongs to field of waste water treatment, more particularly, to a kind for the treatment of by catalytic oxidation of alkali decrement waste water.
Background technology
Alkali reduction be printing and dyeing enterprise in order to improve the performances such as the comfortableness of dacron, flexibility used by produce work
Skill, by carrying out alkali process to terylene, make the ester bond in terylene that a certain degree of hydrolysis occur in alkaline solution, so that
A certain degree of fracture occurs for macromolecular chain, and with the progress of hydrolysis, a certain degree of change also occurs for the form of fiber surface,
Make polyester fiber that there is the performance as silk, obtain the effect of Silk.After alkali deweighting, weight is reduced dacron
About 20%, this few fibers generates para-phthalic sodium and ethylene glycol in the presence of NaOH and is dissolved in water.In addition, in order to add
Speed hydrolysis, will also add some surfactants in alkali lye, allow for alkali deweighting waste liquid as basicity is big, organic concentration
High waste liquid.
Nano zero valence iron (nanoscale Zero-valent Ironn, nano-ZVI) refers to particle diameter yardstick in 1-100nm
Within nulvalent iron particle.Because the diameter of nanometer nulvalent iron particle is smaller, therefore its surface atom accounts for the percentage of total atomic amount
It is bigger, therefore the features such as show bulk effect, skin effect and quantum size effect, particle diameter is 10nm nano zero valence iron
Particle specific surface area is 37 times of common iron powder, has very strong catalysis deoxidization, degradation ability.In recent years, sodium peroxydisulfate is because having
The advantages that friendly of preferably water-soluble, strong oxidizing property and reaction product, turn into one kind for degradable organic pollutant
New oxidants, but Na2S2O8It is relatively stable under normal temperature, oxidability and unobvious, only after the activation such as transition metal, alkali, heat
The very strong potentiometric titrations (SO of oxidisability could be produced4 -, E0=2.6V) and hydroxyl radical free radical (OH, E0=2.8V).
The mechanism of nano zero valence iron activation sodium peroxydisulfate is as follows：
2Fe0+O2+2H2O→2Fe2++4OH-
Fe0+2H2O→Fe2++2OH-+H2
Fe2++S2O8 2-→Fe3++·SO4 -+SO4 2-
Under conditions of strong basicity, S2O8 2-With the OH in alkaline waste water-Reaction produces OH free radicals.Mechanism is as follows：
SO4·-+OH-→·OH+SO4 2-
S2O8 2-→SO4 2-+SO4·-
S2O8 2-+OH-→2SO4 2-+·OH
Chinese invention " a kind of method of Fenton technology processing Alkaline high-strength organic wastewater ", application number
201210298485.8 disclose one kind by adding FeSO again after adding strong acid change wastewater pH4·7H2O processing strong basicities are high
The method of concentration organic wastewater, this method can effectively reduce the organic concentration in waste water, but this method to the pH of waste water will
Ask very high, it is necessary to which the pH regulations of strong basicity waste water are arrived into highly acid, then add FeSO4·7H2O, then by pH regulations to 7.5~
8.5, polyacrylamide (PAM) is finally added, not only cumbersome, reciprocal regulation pH value adds processing cost, and past useless
FeSO is added in water4·7H2O solids can cause Fe2+Loss, produce a large amount of sludge.A kind of Chinese invention " alkali decrement waste water money
Source handling process ", application number 201510255831.8 disclose a kind of alkali decrement waste water recycling treatment process, and this method is first
First it is 2~4 and reacts 5~8h, bottom of pond recycling precipitate terephthalic acid (TPA), supernatant using concentrated sulfuric acid regulation pH value in acid out pond
Liquid enters catalytic oxidation system, in composite catalyst and O2、H2O2Reaction continues 1~2h under being acted on Deng oxidant, then adjusts pH
6~9 and to carry out flocculation sediment, A/O biochemical systems 30~40h of biological reinforced reaction under high salt bacterium existence condition is entered back into.
This method can reclaim the part terephthalic acid (TPA) in waste water, but need repeatedly regulation pH value, equally exist cumbersome, it is necessary to past
Polyphony section pH value, increase processing cost the problems such as.
The content of the invention
The invention aims to overcome to need back and forth to adjust pH value, processing cost height etc. existing for prior art and lack
Fall into, there is provided a kind for the treatment of by catalytic oxidation of alkali decrement waste water.This method uses liquid-phase reduction sedimentation, by being born with charcoal
Nano zero-valence ferrous metal is carried as catalyst, catalytic activation persulfate produces potentiometric titrations, and sulphur in the basic conditions
Acid group radical conversion is hydroxyl radical free radical, forms and strengthens advanced oxidation system.Hardly degraded organic substance in waste water is mainly
Attacked by free radical and disconnect loop configuration, be finally mineralized to form small molecule inorganic matter.This method technique is simple, oxidation efficiency
The treatment by catalytic oxidation of high, non-secondary pollution alkali decrement waste water.
Above-mentioned purpose of the present invention is achieved by the following technical programs：
A kind for the treatment of by catalytic oxidation of alkali decrement waste water, is comprised the following specific steps that：
S1. at 50~70 DEG C, charcoal is placed in nitric acid and soaked, and rinsed to pH stable；
S2. by FeSO4·7H2O is dissolved in deionized water, is obtained mixed solution after adding absolute ethyl alcohol, is added into mixed solution
Enter charcoal, lasting stirring makes charcoal be sufficiently mixed with solution；
S3. under the protection of inert gas, KBH is added dropwise to step S2 resulting solutions4Solution, it is aged after being added dropwise to complete anti-
Should, scrubbed and drying process, charcoal load nano zero-valence iron catalyst is made；
S4. charcoal load nano zero-valence iron catalyst is added in alkali decrement waste water, adds Na2S2O8, in normal temperature bar
Reacted under part, take out reacted mixed liquor measure CODcr concentration.
Preferably, the particle size of charcoal described in step S1 is 50~100 mesh, the concentration of the nitric acid for 0.5~
2mol/L, the time of the immersion is 6~8h, and the pH value is 7~7.5.
Preferably, the mass volume ratio of charcoal and nitric acid described in step S1 is (0.5~1)：3g/mL.
Preferably, FeSO described in step S24·7H2O and the mass volume ratio of deionized water are (0.5~1)：4g/mL,
The deionized water and the volume ratio of absolute ethyl alcohol are (1~2)：4, the mass volume ratio of the charcoal and mixed solution for (1~
2)：40g/mL, the time of the stirring is 1~2h.
Preferably, step S2 resulting solutions and KBH described in step S34The volume ratio of solution is (2~3)：1, the wood
The mass ratio of charcoal and iron is (2.5~10) in charcoal load nano zero-valence iron catalyst：1.
Preferably, inert gas described in step S3 is nitrogen, argon gas or helium, time of the ageing reaction for 1~
2h, the solution of the washing is deionized water and absolute ethyl alcohol.
Preferably, the mass volume ratio of the load nano zero-valence iron catalyst of charcoal described in step S4 and alkali decrement waste water is
(0.01~0.03)：50g/mL, the charcoal load nano zero-valence iron catalyst and Na2S2O8Mass ratio be (1~3)：(3~
5)。
Preferably, the time reacted described in step S4 is 2~4h.
Compared with prior art, the invention has the advantages that：
1. nano zero valence iron is supported on charcoal by the present invention, the defects of can not only overcoming nano zero valence iron easily to reunite,
And because charcoal specific surface area is big, adsorption site is more, the organic matter in waste water efficiently can be adsorbed to nano zero-valence iron surface,
Improve catalytic efficiency.
2. catalyst of the present invention uses Fe0Original position provides Fe2+Activate S2O8 2-, produce the SO with strong oxidizing property4 ·-, it is non-equal
Phase activator Fe0Can slowly, discharge Fe in the solution step by step2+, control the Fe in solution2+Amount, so as to reduce
Surplus Fe2+With SO4 ·-The probability of side reaction occurs, improves the utilization rate of persulfate.
3. the present invention is swashed using the nanometer iron metal ion loaded in the strong basicity and charcoal of waste water to persulfate
Living, course of reaction need not adjust the pH value of waste water, high to the oxidation efficiency of alkali decrement waste water, and CODcr removal effects are good, processing
The cost of waste water is low.
Embodiment
Present disclosure is further illustrated with reference to specific embodiment, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagent, method and apparatus.
Embodiment 1
1. the charcoal of 100 mesh is placed in 1mol/L salpeter solutions, after soaking 8h in 60 DEG C of water-baths, cleaned with distilled water
No longer change to pH value, dried at 105 DEG C；
2. weigh 4.96g FeSO4·7H2O is dissolved in 20mL deionized waters, treats FeSO4·7H280ml is added after O dissolvings
Absolute ethyl alcohol adds 5g charcoals into mixed solution as dispersant, persistently stirred using magnetic stirring apparatus 1h make charcoal with it is molten
Liquid is sufficiently mixed.
3. 50mlKBH is at the uniform velocity added dropwise with the speed of 1-2 drops per second dropwise to mixed liquor under nitrogen protection4Solution.It is added dropwise
After the completion of ageing reaction 1h, then under nitrogen protection respectively with deionized water and absolute ethyl alcohol wash charcoal load nano zero-valence
Iron for several times, is finally dried using vacuum drying chamber, and the mass ratio that charcoal and iron is made is 5：1 catalyst seal saves backup.
4. adding 0.06g charcoals load nano zero-valence iron catalyst in per 100ml alkali decrement waste waters, 0.1g is added
Na2S2O8, the concussion reaction 2h of circling round is placed in oscillator under 25 DEG C of normal temperature conditions.
5. the alkali decrement waste water after oxidation processes is stood into 15min, supernatant is taken to determine its CODcr.
(CODcr bichromate indexes, it is to use potassium bichromate conduct using rapid sealing Catalytic digestion method measure CODcr
The chemical oxygen consumption (COC) that oxidant determines).Comprise the following steps that：
Testing liquid is placed in 25ml heating tubes, 1ml screening agents is added and is mixed.Add 3ml digestion solutions and 5ml catalysis
Agent, 165 DEG C of resolution 25min, is demarcated after cooling with iron ammonium sulfate.Claim 120 DEG C of drying 2h using rapid sealing Catalytic digestion method
Potassium bichromate standard liquid (concentration 0.1mol/L), claim 39.2g (NH4)2Fe(SO4)2·6H2O, which adds the 20ml concentrated sulfuric acids, to be determined
Hold standby to 1000ml volumetric flasks；
Digestion solution：19.6g potassium bichromates are weighed, 50g alums, 10g ammonium molybdates, water is dissolved in and adds the dense sulphur of 200ml
Acid is settled to 1000ml；Catalyst：Ag2SO4(8.8g)-H2SO4(1000ml)；Phenanthroline indicator：Claim 0.695g
FeSO4·7H2The dissolving of O and 1.4850g phenanthrolines is settled to 100ml, is stored in standby in brown bottle；Screening agent：Claim 10.0g
HgSO4, it is dissolved in the sulfuric acid of 100ml 10%.
Experimental result CODcr drops to 978mg/L, clearance 65.1% by 2800mg/L.
Embodiment 2
1. the charcoal of 100 mesh is placed in 2mol/L salpeter solutions, after soaking 8h in 50 DEG C of water-baths, cleaned with distilled water
No longer change to pH value, dried at 105 DEG C；
2. weigh 2.48g FeSO4·7H2O is dissolved in 20mL deionized waters, treats FeSO4·7H280ml is added after O dissolvings
Absolute ethyl alcohol adds 2.5g charcoals into mixed solution as dispersant, persistently stirred using magnetic stirring apparatus 2h make charcoal with
Solution is sufficiently mixed.
3. 50mlKBH is at the uniform velocity added dropwise with the speed of 1-2 drops per second dropwise to mixed liquor under nitrogen protection4Solution.It is added dropwise
After the completion of ageing reaction 1h, then under nitrogen protection respectively with deionized water and absolute ethyl alcohol wash charcoal load nano zero-valence
Iron for several times, is finally dried using vacuum drying chamber, and the mass ratio that charcoal and iron is made is 5：1 catalyst seal saves backup.
4. adding 0.02g charcoals load nano zero-valence iron catalyst in per 100ml alkali decrement waste waters, 0.1g is added
Na2S2O8, the concussion reaction 2h of circling round is placed in oscillator under 25 DEG C of normal temperature conditions.
5. the alkali decrement waste water after oxidation processes is stood into 15min.
Using the method for testing in embodiment 1, supernatant is taken to determine its CODcr.CODcr is dropped to by 2800mg/L
1016mg/L, clearance 63.7%.
Embodiment 3
1. the charcoal of 50 mesh is placed in 1mol/L salpeter solutions, after soaking 6h in 70 DEG C of water-baths, cleaned with distilled water
No longer change to pH value, dried at 105 DEG C；
2. weigh 4.96g FeSO4·7H2O is dissolved in 20mL deionized waters, treats FeSO4·7H280ml is added after O dissolvings
Absolute ethyl alcohol adds 2.5g charcoals into mixed solution as dispersant, persistently stirred using magnetic stirring apparatus 2h make charcoal with
Solution is sufficiently mixed.
3. 33mlKBH is at the uniform velocity added dropwise dropwise to mixed liquor under nitrogen protection4Solution.Ageing reaction 1h after being added dropwise to complete,
Then charcoal load nano zero valence iron is washed for several times with deionized water and absolute ethyl alcohol respectively under nitrogen protection, finally using true
Empty drying box drying, the mass ratio that charcoal and iron is made is 2.5：1 catalyst seal saves backup.
4. adding 0.02g charcoals load nano zero-valence iron catalyst in per 100ml alkali decrement waste waters, 0.06g is added
Na2S2O8, the concussion reaction 3h of circling round is placed in oscillator under 25 DEG C of normal temperature conditions.
5. the alkali decrement waste water after oxidation processes is stood into 15min.
Supernatant is taken to determine its CODcr, CODcr is the chemical oxygen consumption (COC) determined using potassium bichromate as oxidant,
That is bichromate index.CODcr drops to 998mg/L, clearance 64.4% by 2800mg/L.
Embodiment 4
1. the charcoal of 50 mesh is placed in 0.5ml/L salpeter solutions, after soaking 8h in 60 DEG C of water-baths, cleaned with distilled water
No longer change to pH value, dried at 105 DEG C；
2. weigh 2.48g FeSO4·7H2O is dissolved in 20mL deionized waters, treats FeSO4·7H280ml is added after O dissolvings
Absolute ethyl alcohol adds 5g charcoals into mixed solution as dispersant, persistently stirred using magnetic stirring apparatus 1h make charcoal with it is molten
Liquid is sufficiently mixed.
3. 50mlKBH is at the uniform velocity added dropwise dropwise to mixed liquor under nitrogen protection4Solution.Ageing reaction 1h after being added dropwise to complete,
Then charcoal load nano zero valence iron is washed for several times with deionized water and absolute ethyl alcohol respectively under nitrogen protection, finally using true
Empty drying box drying, the mass ratio that charcoal and iron is made is 10：1 catalyst seal saves backup.
4. adding 0.06g charcoals load nano zero-valence iron catalyst in per 100ml alkali decrement waste waters, 0.06g is added
Na2S2O8, the concussion reaction 4h of circling round is placed in oscillator under 25 DEG C of normal temperature conditions.
5. the alkali decrement waste water after oxidation processes is stood into 15min.
Using the method for testing in embodiment 1, supernatant is taken to determine its CODcr.CODcr is dropped to by 2800mg/L
1080mg/L, clearance 61.4%.
Hardly degraded organic substance from embodiment 1-3 as can be seen that the present invention can effectively degrade in alkali decrement waste water, institute
It is ring-type type organic to state organic matter, including phenyl ring class, to phenyl ring class, lactonic ring class and/or condensed ring type organic；The waste water
PH value be 10~12, the CODcr values of the waste water are 2000~5000.The present invention can improve its biodegradability, and react
Journey is carried out at normal temperatures, and reaction condition is simple, and catalyzing oxidizing degrading pollutant is reacted substantially in 2 hours completely, without secondary dirt
Dye, the Practical Project value of this method are high.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind for the treatment of by catalytic oxidation of alkali decrement waste water, it is characterised in that comprise the following specific steps that：
S1. at 50~70 DEG C, charcoal is placed in nitric acid and soaked, and rinsed to pH stable；
S2. by FeSO4·7H2O is dissolved in deionized water, obtains mixed solution after adding absolute ethyl alcohol, wood is added into mixed solution
Charcoal, stirring make charcoal be sufficiently mixed with solution；
S3. under the protection of inert gas, KBH is added dropwise to step S2 resulting solutions4Solution, reaction is aged after being added dropwise to complete, through washing
Wash and drying process, obtained charcoal load nano zero-valence iron catalyst；
S4. charcoal load nano zero-valence iron catalyst is added in alkali decrement waste water, adds Na2S2O8, under normal temperature condition
Reaction, take out reacted mixed liquor measure CODcr concentration.
2. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S1
The particle size of charcoal is 50~100 mesh, and the concentration of the nitric acid is 0.5~2mol/L, and the time of the immersion is 6~8h,
The pH value is 7~7.5.
3. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S1
The mass volume ratio of charcoal and nitric acid is (0.5~1)：3g/mL.
4. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S2
FeSO4·7H2O and the mass volume ratio of deionized water are (0.5~1)：4g/mL.
5. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S2
Deionized water and the volume ratio of absolute ethyl alcohol are (1~2)：4, the mass volume ratio of the charcoal and mixed solution is (1~2)：
40g/mL, the time of the stirring is 1~2h.
6. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S3
Step S2 resulting solutions and KBH4The volume ratio of solution is (2~3)：1.
7. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S3
The mass ratio of charcoal and iron is (2.5~10) in the charcoal load nano zero-valence iron catalyst：1.
8. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S3
Inert gas is nitrogen, argon gas or helium, and the time of the ageing reaction is 1~2h, and the solution of the washing is deionized water
And absolute ethyl alcohol.
9. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that described in step S4
It is (0.01~0.03) that charcoal, which loads nano zero-valence iron catalyst and the mass volume ratio of alkali decrement waste water,：50g/mL, the wood
Charcoal loads nano zero-valence iron catalyst and Na2S2O8Mass ratio be (1~3)：(3~5).
10. the treatment by catalytic oxidation of alkali decrement waste water according to claim 1, it is characterised in that institute in step S4
The time for stating reaction is 2~4h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627250A (en) * | 2019-08-15 | 2019-12-31 | 广东工业大学 | Advanced oxidation-alkali regulation precipitation combined method for treating EDTA-Cu wastewater |
| CN114307964A (en) * | 2022-01-17 | 2022-04-12 | 合肥学院 | Method for preparing iron-nitrogen-doped biochar functional material based on waste paper box and application |
-
2017
- 2017-09-26 CN CN201710879864.9A patent/CN107628665A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627250A (en) * | 2019-08-15 | 2019-12-31 | 广东工业大学 | Advanced oxidation-alkali regulation precipitation combined method for treating EDTA-Cu wastewater |
| CN114307964A (en) * | 2022-01-17 | 2022-04-12 | 合肥学院 | Method for preparing iron-nitrogen-doped biochar functional material based on waste paper box and application |
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Application publication date: 20180126 |