CN103359820A - Method for treatment on wastewater by adopting oil refining waste catalyst for catalytic oxidation - Google Patents
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Abstract
The invention discloses a method for treatment on wastewater by adopting an oil refining waste catalyst for catalytic oxidation. The method comprises the following steps of: performing mixing treatment on the wastewater to be treated, the oil refining waste catalyst and an oxidant to enable the B/C of the wastewater after treatment to be more than 0.3, and performing solid-liquid separation on the wastewater after treatment, wherein the oxidant can oxidize organic matters in the wastewater, and the oil refining waste catalyst can catalyze the oxidation of the organic matters in the wastewater. According to the wastewater treatment method provided by the invention, the oil refining waste catalyst is utilized for promoting the organic matters in the wastewater to be oxidized by the oxidant, thus the oxidation effect against the organic matters in the wastewater is significantly improved, the COD (chemical oxygen demand) value of the wastewater is reduced more effectively, and the biodegradability of the wastewater after treatment is further improved.
Description
Technical field
The present invention relates to a kind of method that adopts oil refining waste catalyst catalytic oxidation treatment waste water.
Background technology
Catalyzer plays irreplaceable vital role in the evolution of chemical industry.At present, 90% chemical engineering process need to use catalyzer.The various commercial catalystss that the whole world has been succeeded in developing are more than 2000 kinds, chemical catalyst is the core of Chemical Engineering Technology, catalyzer occupies considerable status in Chemical Manufacture, especially in oil refining enterprise, more than 50% of Industrial Catalysis dosage that the whole world that accounts for the catalytic amount that uses comes into operation every year, and catalytic oxidizing equipment is the use rich and influential family of catalyzer in oil refining enterprise.
In catalytic cracking unit, after catalyzer used the regular hour, the activity of catalyzer can descend, and for guaranteeing the activity of catalyzer, usually need to lay down the partially catalyzed agent from device, and this part catalyzer is spent catalyst.
In process of production, catalytic cracking unit can produce a large amount of spent catalyst, usually, the crude oil that every processing is 1,000,000 tons, the spent catalyst that catalytic cracking unit produces is the 700-1000 ton.At present, usually will carry out landfill disposal as " danger is useless " material for these spent catalyst, existing so very high security landfill cost wasted again resource, thereby the resource utilization of spent catalyst becomes problem demanding prompt solution.
CN1814556A discloses a kind of method of utilizing spent catalyst to dispose of sewage, the method comprises that the sorbent material that will contain oil refining waste catalyst fully contacts with sewage, sorbent material is adsorbed the organism in the sewage, described oil refining waste catalyst is made by molecular sieve, clay, binding agent, and specific surface area is 100-300m
2/ g, pore volume are 0.1-0.4ml/g; Take the gross weight of catalyzer as benchmark, Al
2O
3Content be the heavy % of 45-70, SiO
2Content be the heavy % of 25-50, P
2O
5Content be the heavy % of 0.2-4, Fe
2O
3Content be the heavy % of 0-0.5, Na
2O, MgO, K
2O, CaO, TiO
2, Re
2O
3Total content be the heavy % of 3-8.The method mainly is the organism that utilizes in the spent catalyst absorption waste water, thereby reaches the purpose that reduces COD value of waste water.But the method is only suitable for processing the waste water of lower concentration, and the method is the method that a kind of pollutent shifts, and can not reduce the gross contamination thing in the environment.
CN1704350A discloses a kind of method of utilizing spent catalyst to prepare polymeric basic aluminum silicate-sulphate flocculent, the method comprises that (acid is 5-15 with the weight liquid-solid ratio of described spent catalyst: be reaction 1-2 hour under 80-100 ℃ the condition in temperature of reaction 1) with 3% sulfuric acid and spent catalyst, direct sour molten heavy-oil catalytic spent catalyst, then using last slag and the sodium hydroxide of 5-20% (the weight liquid-solid ratio of alkali and slag is 10: 1) is reaction 1-2 hour under 80-100 ℃ the condition in temperature of reaction, produce silicate, at last aluminium salt and silicate polymerization are made liquid polymeric aluminum sulfate silicate.The method mainly is to utilize the heavy oil spent catalyst to prepare the macromolecular compound polymeric basic aluminum silicate-sulphate flocculent, and the shortcoming of the method is that acid, quantity of alkali consumption are large, and has the problem of secondary pollution.
Summary of the invention
The object of the present invention is to provide and a kind ofly can effectively utilize oil refining waste catalyst to waste water, the waste water that produces in the oil production that particularly the COD value is higher and/or the petroleum refining process is processed, with the COD value of effective reduction waste water, and the method for the stable employing oil refining waste catalyst catalytic oxidation treatment waste water for the treatment of effect.
The disclosed method of CN1814556A mainly is the organism that utilizes in the spent catalyst absorption waste water, after reaching capacity, catalyzer absorption also needs the organic impurities of absorption is rinsed out from catalyzer, not only need a large amount of wash-down waters, and the organic impurities of absorption just is shifted out from waste water, being rinsed water takes away, can not reach the purpose that reduces pollutent total in the environment, and, because the adsorptive power of described spent catalyst is limited, therefore, the method is not suitable for the higher waste water of organic content is processed.
Although the activity of spent catalyst can't satisfy the needs that oil refining is produced less than fresh dose, but, the present inventor finds, itself still has certain activity described oil refining waste catalyst, when pending waste water and described oil refining waste catalyst and oxygenant are carried out combination treatment, can utilize well the active accelerating oxidation agent of oil refining waste catalyst to the oxidation of waste water, particularly the waste water that produces in the higher oil production of oxidation COD value and/or the petroleum refining process played good catalysed promoted effect.
To achieve these goals, the invention provides a kind for the treatment of process of waste water, wherein, the method comprises carries out combination treatment with pending waste water and oil refining waste catalyst and oxygenant, so that the B/C of processed waste water is＞0.3, and the waste water after will processing carries out solid-liquid separation; The organism of described oxygenant in can oxidized waste water, described oil refining waste catalyst can catalysis waste water in organic oxidation.
The method of employing oil refining waste catalyst catalytic oxidation treatment waste water provided by the invention is carried out combination treatment with pending waste water and oil refining waste catalyst and oxygenant, utilize oil refining waste catalyst to the organic catalysed oxidn in the waste water, Effective Raise organic oxidation effectiveness in the waste water, particularly more remarkable for the treatment effect of the waste water that produces in oil production and/or the petroleum refining process.As according to the method that adopts embodiment 1 and Comparative Examples 1 to waste water carry out the B/C of processed waste water and COD value more as can be known, employing of the present invention utilizes oxygenant waste water to be carried out the effect of oxidation under the method for utilizing oxygenant to wastewater treatment under the catalysis of oil refining waste catalyst has significantly improved catalysis at the heterogeneous catalyst of routine, thereby biodegradability that can more effective raising processed waste water, and reduce the COD value of waste water.In addition, method of wastewater treatment of the present invention adopts the treatment process of the treatment of wastes with processes of wastes against one another, when obtaining good economical effectiveness, also has good social benefit and environmental benefit.
Other features and advantages of the present invention will partly be described in detail in embodiment subsequently.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that embodiment described herein only is used for description and interpretation the present invention, is not limited to the present invention.
According to the present invention, the method of described employing oil refining waste catalyst catalytic oxidation treatment waste water comprises carries out combination treatment with pending waste water and oil refining waste catalyst and oxygenant, so that the B/C of processed waste water is＞0.3, and the waste water after will processing carries out solid-liquid separation; The organism of described oxygenant in can oxidized waste water, described oil refining waste catalyst can catalysis waste water in organic oxidation.
According to the present invention, as long as pending waste water and oil refining waste catalyst and oxygenant are carried out the consumption of the condition of combination treatment and oil refining waste catalyst and oxygenant so that the B/C of the waste water after processing＞0.3.
In the present invention, described oxygenant can carry out oxidation with the impurity such as organism in the water, therefore, the oxygenizement of described oxygenant not only can reduce the COD of waste water effectively, larger molecular organics can also be decomposed into the biodegradability that small organic molecule improves waste water.
According to the present invention, as long as the consumption of the condition of wastewater treatment and oxygenant and catalyzer can provide the biodegradability of waste water, that is, satisfy the B/C make the waste water after the processing that obtains＞0.3 and get final product.Therefore, the selectable range of the consumption of described oxygenant and described oil refining waste catalyst is wider, and can suitably regulate according to the B/C value of pending waste water, as long as can play so that the abundant oxygenolysis of the impurity such as organism in the waste water, and the B/C value that satisfies processed waste water gets final product.Under the preferable case, the mass concentration ratio of oxygenant and waste water COD is 0.01-10: 1, and more preferably in the situation, the mass concentration ratio of oxygenant and waste water COD is 0.05-5: 1, under the most preferred case, the mass concentration ratio of oxygenant and waste water COD is 0.1-2: 1.Under the preferable case, the mass ratio of described oxygenant and described oil refining waste catalyst is 1: 0.1-100; More preferably in the situation, the mass ratio of described oxygenant and described catalyzer is 1: 0.5-50; Under the most preferred case, the mass ratio of described oxygenant and described catalyzer is 1: 1-20.
In the present invention, organic quality can represent with the chemical oxygen demand (COD) (COD) of waste water in the described waste water, COD refers under certain conditions, when adopting certain strong oxidizer to process water sample, the oxidant content that consumes, it is what a index of reducing substances (being mainly organism) in the expression water.Can be understood as so, is the waste water of 1mg/L corresponding to the COD value, and the consumption of oxygenant is 0.01-10mg/L, is preferably 0.05-5mg/L, more preferably 0.1-2mg/L.
According to the present invention, described oxygenant can be this area various oxygenants that the organism in the water etc. can be carried out oxidation commonly used, under the preferable case, described oxygenant can be selected from one or more in hydrogen peroxide, ozone, persulphate, hypochlorite, dioxide peroxide and the chlorine, more preferably hydrogen peroxide.
According to the present invention, described oil refining waste catalyst can catalysis waste water, organic the efficient oxidation in the waste water that produces in the oil production that particularly catalysis COD value is higher and/or the petroleum refining process, consisting of of the oil refining waste catalyst that adopts among the present invention is conventionally known to one of skill in the art, under the preferable case, take the gross weight of described oil refining waste catalyst as benchmark, the content of aluminium sesquioxide is the 45-55 % by weight, the content of silicon-dioxide is the 35-45 % by weight, the content of lanthanum trioxide is the 0.8-1.5 % by weight, the content of cerium oxide is the 1.7-2.5 % by weight, the content of nickel oxide is the 0.5-2.5 % by weight, the content of vanadium dioxide is the 0.3-1 % by weight, and the content of ferric oxide is the 0.5-2.5 % by weight.
According to the present invention, in order can also to play the effect of absorption when utilizing oil refining waste catalyst that waste water is carried out catalyzed oxidation, under the preferable case, the specific surface area of described oil refining waste catalyst is 100-300m
2/ g, pore volume are 0.1-0.4ml/g.
According to the present invention, the condition of described combination treatment generally comprises the temperature and time of combination treatment.
Wherein, the selectable range of the temperature of described combination treatment is wider, usually can be for carrying out under to 40 ℃ at normal temperature (such as 10 ℃).In addition, the present invention was not particularly limited the time of combination treatment, as long as the B/C of the waste water after the processing that can guarantee to obtain＞0.3, and can adjust according to the COD value of pending waste water, generally, the time of described combination treatment can be 5-600 minute, is preferably 10-300 minute, more preferably 30-120 minute.
According to the present invention, the mode of described combination treatment is that waste water is mixed with oxygenant and oil refining waste catalyst, and under the preferable case, in order to make the catalyzed oxidation better effects if to pending waste water, described combination treatment is under agitation carried out.In addition, the addition sequence of described oxygenant, oil refining waste catalyst and to add the selectable range of mode wider under the preferable case, under agitation, adds oxygenant in the waste water and oil refining waste catalyst can make better processing effect successively.
According to the present invention, the method of the waste water after processing being carried out solid-liquid separation can be the method for the various solid-liquid separation of this area routine, for example, the methods such as gravity settling, centrifugation or filtration, its concrete operation method and condition are conventionally known to one of skill in the art.For example, the temperature of described solid-liquid separation can be normal temperature (10-40 ℃), as long as the time of solid-liquid separation can guarantee that abundant separating impurity is with the requirement of the B/C that satisfies processed waste water, the lower COD value that more preferably satisfies processed waste water requires to get final product, generally, the time of solid-liquid separation can be 5-1200 minute, is preferably 10-800 minute, more preferably 60-600 minute.
Method of the present invention goes for the processing of various waste water, is particularly suitable for processing the high density, the organic wastewater with difficult degradation thereby that produce in oil production and/or the petroleum refining process, for example, and the B/C of described pending waste water＜0.3, preferred B/C＜0.2; The COD of described pending waste water can be 60-1500mg/L, even can be up to 200-10000mg/L.
More than describe preferred implementation of the present invention in detail; but the present invention is not limited to the detail in the above-mentioned embodiment, in technical conceive scope of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Need to prove in addition, each concrete technical characterictic described in above-mentioned embodiment in reconcilable situation, can make up by any suitable mode, for fear of unnecessary repetition, the present invention is to the no longer separately explanation of various possible array modes.
In addition, also can carry out arbitrary combination between the various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
The below will further describe in detail embodiments of the invention.
Among the following embodiment, the measuring method of the COD of waste water is dichromate titration (GB11914-89), and the measuring method of the BOD of waste water is dilution inoculation method (GB/T 7488-1987).
Among the following embodiment, the specific surface area of oil refining waste catalyst and the measuring method of pore volume are respectively: measure the specific surface area of oil refining waste catalyst according to the BET specific area measuring method of GB.T 19587-2004, (available from Beijing gold dust spectrum Science and Technology Ltd.: V-Sorb 2800P) (stationary method) measures the pore volume of oil refining waste catalyst to adopt the pore volume determinator.
Embodiment 1
Present embodiment is used for illustrating the treatment process of waste water provided by the invention.
Process certain Refinery Coking waste water, the COD of waste water is 530mg/L, and B/C is 0.13.
Used oil refining waste catalyst is specifically composed as follows in the present embodiment: take the gross weight of described catalyzer as benchmark, the content of aluminium sesquioxide is 52.6 % by weight, the content of silicon-dioxide is 40.8 % by weight, the content of lanthanum trioxide is 1.2 % by weight, the content of cerium oxide is 2.3 % by weight, ferric oxide 1.2 % by weight, the content of nickel oxide are 1.5 % by weight, and the content of vanadium oxide is 0.4 % by weight; The specific surface area of described oil refining waste catalyst is 150-250m
2/ g, pore volume are 1.6-3ml/g.
400 milliliters of above-mentioned pending waste water, add successively the 1.6g mass percent concentration in the waste water and be 5% hydrogen peroxide and the above-mentioned oil refining waste catalyst of 0.6g, combination treatment is 60 minutes under the rotating speed of 400r/min, and standing sedimentation 120 minutes is got supernatant liquor and carried out index analysis.The COD of processed waste water is 310mg/L, and B/C is 0.38.
Embodiment 2
Present embodiment is used for illustrating the treatment process of waste water provided by the invention.
Process certain oil wastewater with PAM, the COD of waste water is 267mg/L, and the B/C of waste water is 0.08.
Used oil refining waste catalyst is specifically composed as follows in the present embodiment: take the gross weight of described catalyzer as benchmark, the content of aluminium sesquioxide is 55 % by weight, the content of silicon-dioxide is 36.6 % by weight, the content of lanthanum trioxide is 1.5 % by weight, the content of cerium oxide is 2.5 % by weight, ferric oxide 1.9 % by weight, the content of nickel oxide are 1.7 % by weight, and the content of vanadium oxide is 0.8 % by weight; The specific surface area of described oil refining waste catalyst is 150-250m
2/ g, pore volume are 0.15-0.35ml/g.
400 milliliters of above-mentioned pending waste water, add successively the 3.56g mass percent concentration in the waste water and be 3% hydrogen peroxide and the above-mentioned oil refining waste catalyst of 0.267g, combination treatment is 80 minutes under the rotating speed of 400r/min, and standing sedimentation 180 minutes is got supernatant liquor and carried out index analysis.The COD of processed waste water is 120mg/L, and B/C is 0.35.
Embodiment 3
Present embodiment is used for illustrating the treatment process of waste water provided by the invention.
Method according to embodiment 1 is processed waste water, and different is: add 0.01g Sodium Persulfate and 0.15g oil refining waste catalyst in waste water, combination treatment is 60 minutes under the rotating speed of 600r/min, and standing sedimentation 120 minutes is got supernatant liquor and carried out index analysis.The COD of processed waste water is 380mg/L, and B/C is 0.33.
Embodiment 4
Present embodiment is used for illustrating the treatment process of waste water provided by the invention.
Method according to embodiment 1 is processed waste water, and different is: add 0.106g clorox and 1g oil refining waste catalyst successively in waste water, combination treatment is 90 minutes under the rotating speed of 600r/min, and standing sedimentation 180 minutes is got supernatant liquor and carried out index analysis.The COD of processed waste water is 290mg/L, and B/C is 0.4.
Embodiment 5
Present embodiment is used for illustrating the treatment process of waste water provided by the invention.
Method according to embodiment 1 is processed waste water, and different is: pending waste water is wastewater from chemical industry, and the COD value is that 840, B/C is 0.18, and the COD of processed waste water is 520mg/L, and B/C is 0.3.
Embodiment 6
Present embodiment is used for illustrating the treatment process of waste water provided by the invention.
Method according to embodiment 1 is processed waste water, different is: the COD of waste water is 5000mg/L, B/C is 0.08,400 milliliters of above-mentioned pending waste water, add successively the 80g mass percent concentration in the waste water and be 5% hydrogen peroxide and the above-mentioned oil refining waste catalyst of 10g, combination treatment is 60 minutes under the rotating speed of 400r/min, and standing sedimentation 120 minutes is got supernatant liquor and carried out index analysis.The COD of processed waste water is 840mg/L, and B/C is 0.32.
Comparative Examples 1
This Comparative Examples is used for the reference method of explanation wastewater treatment.
Method according to embodiment 1 is carried out oxide treatment to Refinery Coking waste water, different is, what adopt is heterogeneous catalyst available from woods China water treatment company, the main component of described catalyzer is: activated carbon content is 93 % by weight, cerium oxide content is 1.5 % by weight, ferric oxide content is 2 % by weight, and vanadium dioxide content is 1.5 % by weight, and cupric oxide content is 2 % by weight; Other oxidizing condition is identical with embodiment 1, and the COD of processed waste water is 435mg/L, and B/C is 0.16.
Can find out that according to the above results the treatment effect of other heterogeneous catalyst catalytic oxidation treatment difficult degradation refinery waters of the employing of Comparative Examples 1 is not satisfactory.Hence one can see that; adopt the method for the catalytic oxidation treatment waste water of oil refining waste catalyst of utilizing of the present invention can significantly improve oxygenant to organic oxidation effectiveness in the waste water; thereby the biodegradability of the more effective raising processed waste water of energy; in addition; adopt the treatment process of the treatment of wastes with processes of wastes against one another, also saved resource and protected environment.
Claims (10)
1. method that adopts oil refining waste catalyst catalytic oxidation treatment waste water, it is characterized in that, the method comprises carries out combination treatment with pending waste water and oil refining waste catalyst and oxygenant, so that the B/C of processed waste water is＞0.3, and the waste water after will processing carries out solid-liquid separation; The organism of described oxygenant in can oxidized waste water, described oil refining waste catalyst can catalysis waste water in organic oxidation.
2. method according to claim 1, wherein, the mass concentration ratio of oxygenant and waste water COD is 0.01-10: 1.
3. method according to claim 2, wherein, the mass concentration ratio of oxygenant and waste water COD is 0.05-5: 1, be preferably 0.1-2: 1.
4. the described method of any one according to claim 1-3, wherein, the mass ratio of described oxygenant and described oil refining waste catalyst is 1: 0.5-50.
5. method according to claim 4, wherein, the mass ratio of described oxygenant and described oil refining waste catalyst is 1: 1-20.
6. the described method of any one according to claim 1-3 and in 5, wherein, described oxygenant is selected from one or more in hydrogen peroxide, ozone, persulphate, hypochlorite, dioxide peroxide and the chlorine.
7. method according to claim 1 or 5, wherein, take the gross weight of described oil refining waste catalyst as benchmark, the content of aluminium sesquioxide is the 45-55 % by weight, and the content of silicon-dioxide is the 35-45 % by weight, and the content of lanthanum trioxide is the 0.8-1.5 % by weight, the content of cerium oxide is the 1.7-2.5 % by weight, the content of nickel oxide is the 0.5-2.5 % by weight, and the content of vanadium dioxide is the 0.3-1 % by weight, and the content of ferric oxide is the 0.5-2.5 % by weight.
8. method according to claim 1, wherein, the method for described solid-liquid separation is selected from one or more in gravity settling, centrifugation and the filtration; The time of solid-liquid separation is 5-1200 minute.
9. the described method of any one according to claim 1-3, wherein, the COD value of described pending waste water is 60-1500mg/L.
10. the described method of any one according to claim 1-3, wherein, described pending waste water is the waste water that produces in oil production and/or the petroleum refining process.
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| CN105562021A (en) * | 2014-10-09 | 2016-05-11 | 中国石油化工股份有限公司 | Catalyst for sodium hypochlorite-based catalytic oxidation of biorefractory waste water and preparation method thereof |
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| CN107442115A (en) * | 2016-05-30 | 2017-12-08 | 中国石化扬子石油化工有限公司 | One kind oil refining waste soda residue wet oxidizing catalyst and preparation method thereof |
| CN108862562A (en) * | 2017-05-09 | 2018-11-23 | 中国石油化工股份有限公司 | Biomembrane suspending carrier and its method of application and biological contact oxidization treatment waste water |
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| CN104138754B (en) * | 2014-06-09 | 2018-07-13 | 西南石油大学 | The catalyst and preparation method thereof of dissolved organic matter in purifying tail gas of diesel vehicles |
| CN105562021B (en) * | 2014-10-09 | 2018-07-03 | 中国石油化工股份有限公司 | Sodium hypochlorite catalysis oxidation difficulty biochemical waste water catalyst and preparation method thereof |
| CN105562021A (en) * | 2014-10-09 | 2016-05-11 | 中国石油化工股份有限公司 | Catalyst for sodium hypochlorite-based catalytic oxidation of biorefractory waste water and preparation method thereof |
| CN104370358B (en) * | 2014-11-13 | 2016-04-20 | 中国石油大学(北京) | Utilize method and the device of oil refining waste catalyst and ozonize oil refining saline sewage |
| CN104370358A (en) * | 2014-11-13 | 2015-02-25 | 中国石油大学(北京) | Method and device for treating oil refining salt-containing sewage by using oil refining waste catalyst and ozone |
| CN105797738A (en) * | 2016-04-08 | 2016-07-27 | 北京今大禹环境技术股份有限公司 | Method for preparing catalyst for catalytic oxidation of ozone from waste catalyst produced during oil refining and catalyst prepared with method and used for catalytic oxidation of ozone |
| CN107442115A (en) * | 2016-05-30 | 2017-12-08 | 中国石化扬子石油化工有限公司 | One kind oil refining waste soda residue wet oxidizing catalyst and preparation method thereof |
| CN107442115B (en) * | 2016-05-30 | 2020-08-11 | 中国石化扬子石油化工有限公司 | Oil refining alkaline residue wet oxidation catalyst and preparation method thereof |
| CN108862562A (en) * | 2017-05-09 | 2018-11-23 | 中国石油化工股份有限公司 | Biomembrane suspending carrier and its method of application and biological contact oxidization treatment waste water |
| CN108862562B (en) * | 2017-05-09 | 2021-12-17 | 中国石油化工股份有限公司 | Biological membrane suspension carrier and application thereof, and method for treating wastewater by biological contact oxidation |
| CN114522699A (en) * | 2022-03-04 | 2022-05-24 | 中国科学院过程工程研究所 | Method for removing surface oil of waste oil refining catalyst |
| CN114522699B (en) * | 2022-03-04 | 2023-10-27 | 中国科学院过程工程研究所 | Method for removing oil on surface of waste oil refining catalyst |
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