CN108706716A - The processing method of itrogenous organic substance in a kind of waste water - Google Patents
The processing method of itrogenous organic substance in a kind of waste water Download PDFInfo
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- CN108706716A CN108706716A CN201810649305.3A CN201810649305A CN108706716A CN 108706716 A CN108706716 A CN 108706716A CN 201810649305 A CN201810649305 A CN 201810649305A CN 108706716 A CN108706716 A CN 108706716A
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/06—Pressure conditions
- C02F2301/066—Overpressure, high pressure
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of processing methods of itrogenous organic substance in waste water, using the Titanium Sieve Molecular Sieve of multi-stage porous as catalyst, promote the oxidation reaction between itrogenous organic substance in oxidant and waste water, itrogenous organic substance in waste water is made to degrade.Compared with the prior art, the advantages of the present invention are as follows：The present invention utilizes the Titanium Sieve Molecular Sieve of multi-stage porous (mesoporous and micropore), it can promote the oxidation reaction in oxidant and waste water between itrogenous organic substance under low pressure and lower temperature, the itrogenous organic substance that property is stablized in waste water can be efficiently removed, and reusable.In addition, by " flocculation de-oiling-catalysis oxidation " combination technique processing, the biochemical property of waste water can effectively improve.
Description
Technical field
The present invention relates to field of waste water treatment, a kind of processing method of itrogenous organic substance in waste water is referred specifically to.
Background technology
Impurity (such as sulfur-bearing, nitrogen, oxygen non-hydrocarbon compound and trace meter etc.) in oil is in process with virtue
The forms such as fragrant same clan's organic matter, mercaptan thio-ether type compounds, ammonia, sulfide have been transferred to water phase, have so as to form difficult to degrade
Poison and the organic wastewater for having peculiar smell.Relative to other impurity in waste water, aromatic organic impurities are more difficult, aromatic
Substance includes mainly oxygen-bearing organic matter such as phenol and its derivative, itrogenous organic substance such as quinolines and pyridine compounds and their, contains
Sulfur organic such as thiophenes and benzene class and its derivative etc., wherein itrogenous organic substance are especially difficult to degrade difficult.Stone
Oily more heavy seeds are more, and the organic wastewater concentration of formation is higher, peculiar smell also becomes apparent from, and the COD of waste water is (following sometimes
Abbreviation COD) value is up to 10000~30000mg/L or more.Nitrogen content is higher in oil, and nitrogenous compound is more in waste water, therefore
The high concentrated organic wastewater intractability bigger generated during high nitrogen processing of heavy oil.Although the high-concentration waste water accounts for oil refining enterprise
The ratio of total wastewater flow rate is little, but due to the high difficult for biological degradation of its concentration, is impacted greatly to the waste water treatment system of oil refining enterprise, if
Be discharged into environment then will cause catastrophic effect to surrounding water, soil.
Currently, be advanced oxidation processes for the effective processing method of the high concentrated organic wastewater of bio-refractory, advanced oxygen
Change method has photocatalytic oxidation, Ozonation, wet oxidation process and Fenton reagent method etc..Photochemical catalytic oxidation is by light and light
Catalyst combines a kind of sophisticated method of the effective degradation of organic substances formed, and high efficiency photocatalyst exploitation is that photochemical catalyst is developed
Emphasis.Ozone (O3) it is a kind of strong oxidizer, catalyst, which is added, in ozone oxidation system can be improved organic matter degradation efficiency, suitable
Catalyst exploitation be the key that one of waste water treatment by ozone oxidation.Wet oxidation process is usually required in high pressure-temperature, and air is deposited
It carries out under the conditions, the efficiency of organic matter degradation greatly improves in the presence of catalyst or required temperature, pressure will be big
Big to reduce, the catalyst for developing resistance to thermal and hydric environment is one of developing direction of Wet Catalytic Oxidation Method.Fenton reagent method is not necessarily to
High temperature and pressure can carry out at normal temperatures and pressures, and the catalytic active substance used in Fenton reagent method is mainly transition gold at present
Belong to ion such as Fe2+, reaction needs in acid condition, to expand pH ranges, the reduction metal ion that Fenton reagent method uses
(such as Fe2+) to water pollution and be easy to catalyst recycling, new Fenton reagent need to be researched and developed.
Invention content
The technical problem to be solved by the invention for the present situation of prior art is to provide a kind of reusable, and
The processing method of itrogenous organic substance in waste water is efficiently removed under low pressure and lower temperature.
Technical solution is used by the present invention solves above-mentioned technical problem：The processing side of itrogenous organic substance in a kind of waste water
Method, it is characterised in that：Using the Titanium Sieve Molecular Sieve of multi-stage porous as catalyst, promote in oxidant and waste water between itrogenous organic substance
Oxidation reaction makes itrogenous organic substance in waste water degrade.
Titanium Sieve Molecular Sieve be it is a kind of with titanium for heteroatomic molecular sieve, there is excellent absorption property, the titanium silicon of multi-stage porous
Molecular sieve can effectively remove the pollutant of different molecular structures size.
Preferably, the multi-stage porous of the Titanium Sieve Molecular Sieve includes micropore and mesoporous, the micropore size is 1.4~
2.2nm, the mesopore pore size are 2.2~6.5nm, and the percentage by volume in the multi-stage porous of the Titanium Sieve Molecular Sieve shared by micropore is
50~80%.The suitable mesoporous of Titanium Sieve Molecular Sieve and micropore size and ratio can ensure mechanical strength etc..
Preferably, the oxidant is hydrogen peroxide (hereinafter referred to as H2O2).Titanium Sieve Molecular Sieve is to H2O2The organic matter of participation
Selective Oxidation has good activity, high selectivity.
Further, the H2O2The H for being 30% for mass fraction2O2Reagent.
Preferably, the processing method of itrogenous organic substance includes the following steps in above-mentioned waste water：Oxidation is added in waste water
The Titanium Sieve Molecular Sieve of agent and multi-stage porous is placed in autoclave, then is sealed, and then heating carries out catalytic oxidation.
Further, the reaction temperature is 100~250 DEG C；The reaction time is 40~90min；The reaction pressure
Less than 40atm.
Further, the reaction temperature is 150~200 DEG C；The reaction time is 50~70min；The reaction pressure
Power is 7~31atm.
Further, the processing method of itrogenous organic substance is further comprising the steps of in the waste water：It is anti-will to participate in catalysis oxidation
Waste water before answering carries out pH adjustings, i.e.,：By adding sulfuric acid solution or sodium hydroxide solution, wastewater pH is adjusted to required
Value.
Further, the wastewater pH after the pH is adjusted is 4~10.
Further, the processing method of itrogenous organic substance is further comprising the steps of in the waste water：By polyaluminium chloride (following letter
Claim PAC) be added in the waste water before participating in catalytic oxidation the de-oiling reaction that flocculate, i.e.,：PAC is added in waste water,
It is stirred again, supernatant liquor is taken after being then allowed to stand.
Further, the reaction temperature is 30~40 DEG C, and the mixing time is 5~15min, and the time of repose is
10~30min.
Compared with the prior art, the advantages of the present invention are as follows：The present invention is divided using the titanium silicon of multi-stage porous (mesoporous and micropore)
Son sieve, can promote the oxidation reaction in oxidant and waste water between itrogenous organic substance under low pressure and lower temperature, can efficiently go
It is and reusable except the itrogenous organic substance that property is stablized in waste water.In addition, by " flocculation de-oiling-catalysis oxidation " combination skill
Art processing, can effectively improve the biochemical property of waste water.
Description of the drawings
Fig. 1 is the conversion ratio of quinoline under different catalytic oxidation systems；
Fig. 2 is the conversion ratio and COD removal rates of quinoline at a temperature of differential responses；
Fig. 3 is the conversion ratio and COD removal rates of quinoline under different pH；
Fig. 4 is the conversion ratio and COD removal rates of quinoline under different oxidizers；
Fig. 5 is the conversion ratio and COD removal rates of quinoline under different catalysts dosage；
Fig. 6 is the conversion ratio and COD removal rates of quinoline under different catalysts reaction times；
Fig. 7 is the COD removal rates of high concentration petroleum wastewater under different catalytic oxidation systems.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail.
The processing method of itrogenous organic substance is as follows in a kind of waste water：Using the Titanium Sieve Molecular Sieve of multi-stage porous as catalyst, promote
Oxidation reaction in oxidant and waste water between itrogenous organic substance makes itrogenous organic substance in waste water degrade.
Titanium Sieve Molecular Sieve be it is a kind of with titanium for heteroatomic molecular sieve, there is excellent absorption property, the titanium silicon of multi-stage porous
Molecular sieve can effectively remove the pollutant of different molecular structures size.
The multi-stage porous of above-mentioned Titanium Sieve Molecular Sieve includes micropore and mesoporous, and aforementioned micropore size is 1.4~2.2nm, in aforementioned
Hole aperture is 2.2~6.5nm, and the percentage by volume in the multi-stage porous of aforementioned Titanium Sieve Molecular Sieve shared by micropore is 50~80%.This
The percent by volume of sample illustrates the quantity of micropore in the multi-stage porous of Titanium Sieve Molecular Sieve far more than mesoporous.
The suitable mesoporous of Titanium Sieve Molecular Sieve and micropore size and ratio have following advantage：
(1) average pore size of mesoporous is about 2.8nm, and the presence of mesoporous has conducive to the diffusion of macromolecular quinoline；
(2) average pore size of micropore is about 1.8nm, and micropore proportion is larger, is conducive to quinoline decomposition product (small molecule
Organic matter) it is further degradable, therefore COD removal rates are higher；
(3) aperture is bigger, can more influence the mechanical strength of Titanium Sieve Molecular Sieve, and general mesopore pore size is 2~50nm, but this hair
Bright mesoporous average pore size is about 2.8nm, is not comparatively especially big, and micropore proportion is more than mesoporous institute accounting
Example so that the mechanical strength of molecular sieve can be protected, and be conducive to recycling and the industrial applications of catalyst.
Wherein above-mentioned oxidant is H2O2, preferably mass fraction be 30% H2O2Reagent.Titanium Sieve Molecular Sieve is to H2O2Ginseng
With organic matter Selective Oxidation have good activity, high selectivity.
The processing method of itrogenous organic substance includes the following steps in above-mentioned waste water：Oxidant and multi-stage porous are added in waste water
Titanium Sieve Molecular Sieve be placed in autoclave, then be sealed, then heating carries out catalytic oxidation.
Wherein above-mentioned reaction temperature is 100~250 DEG C, preferably 150~200 DEG C
The wherein above-mentioned reaction time is 40~90min, preferably 50~70min.
Wherein above-mentioned reaction pressure is less than 40atm, preferably 7~31atm.
Preferably, the processing method of itrogenous organic substance is further comprising the steps of in above-mentioned waste water：It is anti-will to participate in catalysis oxidation
Waste water before answering carries out pH adjustings, i.e.,：By adding sulfuric acid solution or sodium hydroxide solution, wastewater pH is adjusted to required
Value.
Wastewater pH after wherein above-mentioned pH is adjusted is 4~10.
Preferably, the processing method of itrogenous organic substance is further comprising the steps of in above-mentioned waste water：PAC is added to participation to urge
Flocculation de-oiling reaction is carried out in waste water before oxidation, i.e.,：PAC is added in waste water, then is stirred, is then allowed to stand
After take supernatant liquor.
Wherein above-mentioned reaction temperature is 30~40 DEG C.
Wherein above-mentioned mixing time is 5~15min, and above-mentioned time of repose is 10~30min.
Itrogenous organic substance mainly has pyridine (C in petroleum wastewater5H6N, monocycle), aniline (C6H7N, monocycle), indoles (condensed ring,
Hexatomic ring and five-membered ring, C8H7N), quinoline (C9H7N, condensed ring, two hexatomic rings) and quinoline substance, in these itrogenous organic substances
In, fused ring compound is difficult to degrade, therefore the embodiment of the present invention is with quinoline and difficult for biological degradation (BOD5/COD<0.2) highly concentrated
Representative of the petroleum wastewater as organic matter difficult to degrade in petroleum wastewater is spent, the oxidative degradation phenomenon of waste water is studied.
The specific surface area test result of Titanium Sieve Molecular Sieve is as shown in table 1 in comparative example and embodiment.
The specific surface area test result of Titanium Sieve Molecular Sieve in 1 comparative example of table and embodiment
1~A3 of Comparative examples A and reaction condition in embodiment A1~A18 and the performance test results are as shown in table 2.
2 1~A3 of Comparative examples A of table and the reaction condition in embodiment A1~A18 and the performance test results
The N of catalyst after the catalyst that is inactivated after use 8 times in embodiment A18, fresh and roasting2Absorption representation point
The results are shown in Table 3 for analysis.
The N2 absorption tables of catalyst after the catalyst that is inactivated after use 8 times in 3 embodiment A18 of table, fresh and roasting
Levy analysis result
Comparative example B1~B3 and reaction condition in embodiment B1 and the performance test results are as shown in table 4.
4 comparative example B1~B3 of table and the reaction condition in embodiment B1 and the performance test results
Reaction condition and the performance test results in embodiment B2~B7 is as shown in table 5.
Reaction condition in 5 embodiment B2~B7 of table and the performance test results
Note：
In the embodiment of the present invention, reactor volume 500ml, waste water solution 350ml, when reaction system is closed, system
In have the air of 130ml, when reaction temperature is 50 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C reaction pressure be respectively 0.7Mpa,
1.1Mpa,1.3Mpa,2.4Mpa,3.1Mpa；
In the embodiment of the present invention, it is 8 to carry out the pH of quinoline solution and high concentration petroleum wastewater before pH is adjusted, therefore in table
The embodiment that pH is 8 in reaction condition does not carry out pH adjustings；
The performance test results deviation of the same embodiment of the present invention in different experiments group is as caused by experimental error；
In the embodiment of the present invention, the test method of properties is as follows：
(1) quinoline conversion ratio：Quinoline before quinoline conversion ratio=(quinoline concentration after quinoline concentration-reaction before reaction)/reaction
Concentration × 100%, quinoline method for measurement of concentration are spectrophotometry；
(2) COD removal rates：COD value × 100% before COD conversion ratios=(COD value after COD value-reaction before reaction)/reaction,
COD value assay method is potassium dichromate method (rapid-digestion)；
(3)BOD5：Biochemical process (BOD biochemical measurements instrument) on the 5th；
(4) oil content：Infrared spectrophotometer；
(5) specific surface area and Kong Rong：N2Absorption method.
From table 1~4 and Fig. 1~7：
(1) Titanium Sieve Molecular Sieve of multi-stage porous can effectively degrade the compound in quinoline and high concentration petroleum wastewater,
Main cause is：On the one hand, common Titanium Sieve Molecular Sieve, because of only micropore, the larger pollutant of molecular structure (such as quinoline), because
Molecule is into not micropore, and effect is poor, and the Ti -Si zeolite of multi-stage porous can then effectively remove molecular structure in these waste water
Larger pollutant (such as quinoline)；On the other hand, wastewater degradation produces the intermediate product with brown color, intermediate product into
One step is degraded to colourless low molecule organic matter, H2O and CO2, so that the pH value of waste water is reduced, common metal catalyst is easily in acidity
(i.e. not acidproof) is dissolved out under environment, and Titanium Sieve Molecular Sieve is acidproof；
(2) temperature of general Wet Catalytic Oxidation Method processing waste water is 200-280 DEG C, pressure 2-8MPa, and of the invention
Titanium Sieve Molecular Sieve under low pressure (be less than 40atm, about 31atm) and lower temperature (150 DEG C) can efficiently remove what property was stablized
Itrogenous organic substance；
(3) quinoline can get higher degradation effect in the environment of faintly acid, neutrality, alkalescent, show this method
There is stronger adaptability to quinoline solution ph；Degradation efficiency is high in neutral conditions for quinoline, and neutrallty condition is conducive to equipment
Anti-corrosion；
(4) suitable oxidant and catalyst amount may advantageously facilitate the degradation efficiency of quinoline；
(5) crystal phase structure of the molecular sieve after using 8 times does not change in wet oxidation process, and skeleton structure is complete
Property is preferable, and the stability of molecular sieve is preferable；Deactivation cause is mainly carbon deposit, and being calcined in air can activity recovery.
As shown in Table 5：
(1) high concentration emulsifying waste water is by " flocculation de-oiling-catalysis oxidation ", the COD value of waste water from 5600mg/L~
12400mg/L is reduced to 460mg/L~750mg/L, BOD5/ COD is higher than 0.5, and oil content is less than 10mg/L, therefore the waste water has
There is good biochemical property；
(2) when the quinoline for adding 320mg/L in emulsifying waste water, waste water becomes high nitrogen cut oil waste water, waste water warp
" flocculation-catalysis oxidation " is crossed, the COD value of waste water is reduced to 722mg/L~1394mg/L from 6465mg/L~13300mg/L, to the greatest extent
Waste water BOD after pipe de-oiling5The very low (< of/COD value;0.1) after, but by catalysis oxidation, BOD5/ COD value is higher than 0.5, oil at this time
Content is less than 10mg/L, therefore the waste water has good biochemical property；
(3) flocculation de-oiling can effectively reduce oil content, and catalysis oxidation can effectively reduce COD value, by " flocculation is de-
The processing of oil-catalysis oxidation " combination technique, can effectively improve the biochemical property of waste water.
In conclusion the present invention utilizes the Titanium Sieve Molecular Sieve of multi-stage porous (mesoporous and micropore), under low pressure and lower temperature
It can promote the oxidation reaction between itrogenous organic substance in oxidant and waste water, can efficiently remove nitrogenous the having of property stabilization in waste water
Machine object.In addition, by " flocculation de-oiling-catalysis oxidation " combination technique processing, the biochemical property of waste water can effectively improve.
The present invention is not limited to above-mentioned specific implementation mode, all within the spirits and principles of the present invention, made by it is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. the processing method of itrogenous organic substance in a kind of waste water, it is characterised in that：Using the Titanium Sieve Molecular Sieve of multi-stage porous as catalyst,
Promote the oxidation reaction between itrogenous organic substance in oxidant and waste water, itrogenous organic substance in waste water is made to degrade.
2. the processing method of itrogenous organic substance in waste water according to claim 1, it is characterised in that：The Titanium Sieve Molecular Sieve
Multi-stage porous include micropore and mesoporous, the micropore size is 1.4~2.2nm, and the mesopore pore size is 2.2~6.5nm, described
Percentage by volume in the multi-stage porous of Titanium Sieve Molecular Sieve shared by micropore is 50~80%.
3. the processing method of itrogenous organic substance in waste water according to claim 1, it is characterised in that：The oxidant is
H2O2。
4. the processing method of itrogenous organic substance in waste water according to claim 1, it is characterised in that include the following steps：
Oxidant is added in waste water and the Titanium Sieve Molecular Sieve of multi-stage porous is placed in autoclave, then is sealed, then heating carries out
Catalytic oxidation.
5. the processing method of itrogenous organic substance in waste water according to claim 4, it is characterised in that：The reaction temperature is
100~250 DEG C；The reaction time is 40~90min；The reaction pressure is less than 40atm.
6. the processing method of itrogenous organic substance in waste water according to claim 5, it is characterised in that：The reaction temperature is
150~200 DEG C；The reaction time is 50~70min；The reaction pressure is 7~31atm.
7. the processing method of itrogenous organic substance in waste water according to claim 4, it is characterised in that further comprising the steps of：
Waste water before participation catalytic oxidation is subjected to pH adjustings, i.e.,：By adding sulfuric acid solution or sodium hydroxide solution, by waste water
PH is adjusted to required value.
8. the processing method of itrogenous organic substance in waste water according to claim 7, it is characterised in that：After the pH is adjusted
Wastewater pH is 4~10.
9. the processing method of itrogenous organic substance in waste water according to claim 4, it is characterised in that further comprising the steps of：
PAC is added in the waste water before participating in catalytic oxidation and carries out flocculation de-oiling reaction, i.e.,：PAC is added in waste water, then
It is stirred, supernatant liquor is taken after being then allowed to stand.
10. the processing method of itrogenous organic substance in waste water according to claim 9, it is characterised in that：The reaction temperature
It it is 30~40 DEG C, the mixing time is 5~15min, and the time of repose is 10~30min.
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| CN112744905A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Catalytic ozonation treatment method for wastewater |
| WO2023116315A1 (en) * | 2021-12-22 | 2023-06-29 | 中国石油化工股份有限公司 | Titanium silicate molecular sieve, and nano-gold-loaded titanium silicate molecular sieve catalyst and preparation method therefor and use thereof |
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