CN101066828A - Technological process of treating oil-containing sludge with supercritical water oxidation - Google Patents
Technological process of treating oil-containing sludge with supercritical water oxidation Download PDFInfo
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- CN101066828A CN101066828A CN 200710126149 CN200710126149A CN101066828A CN 101066828 A CN101066828 A CN 101066828A CN 200710126149 CN200710126149 CN 200710126149 CN 200710126149 A CN200710126149 A CN 200710126149A CN 101066828 A CN101066828 A CN 101066828A
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Abstract
The present invention discloses technological process of treating oil-containing sludge with supercritical water for oxidation. The technological process relies on that supercritical water is excellent solvent to organic matter and oxygen, so that the organic matter in oil-containing sludge may be oxidized in oxygen-rich homogeneous phase to produce non-toxic inorganic solid, gaseous and liquid product capable of being exhausted to environment. In addition, the reaction at high temperature has very high speed. Therefore, the present invention provides a simple complete effective oil-containing sludge treating method.
Description
Technical field:
The present invention relates to a kind of treatment process of mud, more particularly utilize the characteristics of supercritical water sludge treatment method, be fit to handle various mud, particularly oily sludge.
Background technology:
It is the unit of oil product as raw material or final product that oil field all over the world reaches with oil product, is all undertaking the task of handling a large amount of oil tank bed muds.Oil product storage tank is storing oil product particularly during crude oil, depositing for a long time in the process, heavy oil components such as a small amount of mechanical impurity, the grains of sand, earth, heavy metallic salt and paraffin in the crude oil and bituminous matter can be because of the difference in specific gravity natural subsidence, be accumulated in tank bottom, form not only black but also thick gelatinoid layer, when the regular tank cleaning of at interval 3～6 years (group company of China Petrochemical Industry regulation), must go out it outside the jar clearly, produce the oil tank bed mud, its quantity is generally more than 1% of this tankage, also has to be reported as 2.2%.
Be rich in organism in the oil tank bed mud, composition is very complicated can not directly to be discharged.Along with optimizing with the public of environmental regulation influences the growing interest of HUMAN HEALTH and living environment to Hazardous wastes, force relevant enterprise must take effectively and the measure of environmental protection processing oil tank bed mud.A large amount of heavy oil materials and silt and water form jelly in the oil tank bed mud, and intractability is big, are the environmental protection difficult problems of puzzlement petrochemical industry always.
Summary of the invention:
In order to overcome the deficiency in the background technology, the invention provides a kind of process for treating oil-containing sludge of being convenient to operate, after handling through this method, the oily sludge of complicated component resolves into environmental protection, nontoxic component, can directly drain into environment.
The concrete steps of process for treating oil-containing sludge of the present invention are as follows:
(2) a certain amount of oily sludge is put into reactor, and in reactor, add a certain amount of water;
(2) temperature and the pressure of setting reactor, wherein temperature is: 350 ℃～550 ℃, pressure is the emergent pressure of water: 22MPa～30MPa;
(3) inject oxygenant after heating reaches temperature of reaction;
(4) reaction 0.5min～15min;
(5) the laggard capable gas, liquid, solid three phase separation of reaction.
The described amount that adds entry is calculated according to Martin-time equation:
Wherein, the common form of temperature function is:
F
k(T)＝A
k+B
kT+C
kexp(-5T/T
c)+D
k/T
(k＝2，3，4，5，6，7，8，9)
A, B, C, D equation constant; K member of equation index; P pressure, MPa; The R gas law constant, J/ (molK); The T temperature, K; The V volume, m
3/ mol.
But 2002 the 30th the 50th～55 page of the 6th phases of volume " development Martin-time equation is as the special equation of water " of method of calculation reference literature " chemical engineering ".
Described temperature of reaction is preferably: 380 ℃～500 ℃.
Described oxygenant is oxygen (O
2), air, hydrogen peroxide (H
2O
2) or ozone (O
3) in a kind of.
The amount of described oxygenant is 1～10 times of theoretical oxygen demand.Wherein be preferably 3～6 times.
The cardinal principle of supercritical water oxidation technical finesse oily sludge is to utilize water under the supercritical state condition, and the free-radical oxidn reaction can take place for oily sludge and oxygenant.Under supercritical state, because supercritical water all is fabulous solvent to organism and oxygen, therefore organic oxidation can be carried out in the homogeneous phase of oxygen enrichment, instead would not be restricted because of alternate transfer.High temperature of reaction also makes speed of response accelerate simultaneously, can in seconds reach very high destruction efficient to organism, and react completely thoroughly, the gas (branch that does not have liquid phase and gas phase under supercritical state) that the reaction back produces is discharged by corresponding valve, enter gas-liquid separation device, isolate gas phase and liquid phase, solid phase is directly stayed in the reactor.Wherein the organic carbon in the mud changes into carbonic acid gas (CO
2), hydrogen changes into water (H
2O), chlorine changes into the metal-salt of chlorion, and sulphur and phosphorus change into vitriol and phosphoric acid salt respectively, and nitrogen then changes into nitrogen (N
2) or nitrous oxide (N
2O).
The present invention has following beneficial effect: oily sludge needn't can directly be put into reactor through mechanical treatment among the present invention, saved existing processing oily sludge and must pass through mechanical dehydration, or drying and dehydrating etc. is consuming time, the step that consumes power;
The present invention to the water ratio of oily sludge, oil length without limits, the oily sludge oil length that the present invention handles can be from 2%-100%;
Oily sludge is sent into the supercritical water oxidation device and is carried out oxidizing reaction, after having reacted, carry out the gas, liquid, solid three phase separation, isolated solid phase composition all changes inorganics into by original many organism that include, promptly not moisture also oil-containing not is so can directly drain into environment; The COD value of liquid composition is lower than 50mg/L, contains a spot of CH
3COOH, according to GB 8978-1996 " integrated wastewater discharge standard ", liquid phase can directly be discharged; Gas phase composition is mainly N
2, CO
2And O
2, also having micro-CO, can directly discharge according to GB 16297-1996 " discharge standard of air pollutants ", environment is not polluted.
Though the oily sludge of different areas or heterogeneity storage tank is formed different, after supercritical water oxidation was handled, it was identical that the final product of generation is formed, so this method is suitable for handling each geographic various oily sludges.
Description of drawings:
Fig. 1 is for implementing the process flow diagram of the method for the invention.
1, oxygenant basin; 3, high-pressure pump; 4, reactor oxidant inlet; 5, temperature controller; 6, feed(raw material)inlet valve; 7, whipping appts; 8, supercritical water oxidation still; 9, reactor outlet valve; 10, interchanger; 11, gas-phase product outlet; 12, separator; 13, liquid product outlet
Embodiment:
The invention will be further described below in conjunction with accompanying drawing:
According to technical process shown in Figure 1, a certain amount of oily sludge is directly added supercritical water oxidation still 8 by feed(raw material)inlet valve 6, then water is also directly added supercritical water oxidation still 8 by feed(raw material)inlet valve 6.Oily sludge and water add reactor 8 late gates 4,6,9 Close Alls, reactor 8 is heated, pressurizes, its temperature is controlled by temperature controller 5, temperature control method certainly adopts known any method, pressure-controlling also can adopt known any method, needs whipping appts 7 to stir simultaneously in the time of heating, pressurization; After reaching design temperature and pressure, the amount that needs is added oxygenant adds in the oxidant vessel 1, injects reactor 8 by high-pressure pump 3, reacts.
After reaction reached the scheduled time, the high temperature and high pressure gas in the reactor 8 entered interchanger 10 via valve 9, and then entered separator 12 and separate, and the gas phase after the separation is discharged by valve 11, and liquid phase is discharged by valve 13.
If gas phase is carried out composition analysis, gas, liquid/gas separator 12 are vacuumized before just need entering gas, liquid/gas separator 12 at the gas in the reactor 8, not influenced by air with component, the content of guaranteeing gas.
Promptly oil-containing is not moisture yet for reacted solid phase, though the oily sludge of different areas is formed difference, after supercritical water oxidation was handled, it was identical that the final product of generation is formed, and has all become the inorganics that does not contain harmful ingredients, so can directly take out discharging.
Certainly utilize the method for supercritical water oxidation technical finesse oily sludge to be not limited to adopt foregoing equipment and Controlling System; promptly under the prerequisite that guarantees the desired processing condition of the inventive method, adopt other equipment and Controlling System also within the protection domain of this patent.
The present invention is further illustrated below by embodiment.
Waste discharge of the present invention institute establishing criteria: liquid composition is GB 8978-1996 " integrated wastewater discharge standard ", standard code: liquid phase can directly be discharged COD and is lower than 50mg/L;
Gas phase composition GB 16297-1996 " discharge standard of air pollutants ".
The detection method of liquid phase COD is measured with potassium dichromate process wherein according to GB/T11914-1989 among the present invention.The oily sludge of mentioning in the present embodiment, the pre-treatment step before handling with the supercritical water oxidation method is meant the oily sludge that takes out directly from jar, with the method mud high to oleaginousness of heat alkali liquid washing, reclaim oil ingredient wherein.
The required theoretical oxygen demand of mentioning in the present embodiment of oily sludge complete oxidation, its method of calculation are: according to the water yield and the oily sludge amount that add in the reactor, measure the required theoretical oxygen demand of oily sludge complete oxidation in the reactor with standard GB/T11914-1989 " the mensuration dichromate titration of hydrochemistry oxygen requirement ".Use O
2When making oxygenant, directly multiply by the multiple that will add; Air then removes O again
2Shared percentage ratio in air; Hydrogen peroxide is then according to concentration, density and the 2molH of hydrogen peroxide
2O
2Resolution produces 1molO
2Relation, calculate the O that the 1mL hydrogen peroxide can produce
2Amount is calculated the required in theory dioxygen water yield again, multiply by the dioxygen water yield that multiple draws needs to add reactor again.
The grand celebration oily sludge in two factory's secondary settlement jars that recovers the oil, water content is 56.8%, contain that liquid oil mass is 38.4%, solids content is 4.8%, through after pre-treatment extracts most of liquid oil component, contain liquid oil and be 2.6%, water ratio 80.6%, solids content 16.8%.Oily sludge after handling is sent into the supercritical water oxidation still, and amount of water is 50mL, and reaction pressure is 24MPa, and temperature of reaction is 500 ℃, O
2Make oxygenant, the oxygenant consumption is 3 times of theory demands amount, and the reaction times is 1 minute, handles back gas and analyzes with gas chromatograph: N
2Be 20.6%, CO
2Be 60.8%, O
2Be 18.4%, CO is 0.2%.Handling back liquid COD is 38mg/L, and the pH value is 5.8.Solid phase is not promptly moisture, yet oil-containing not.According to gas phase, liquid phase and solid phase waste discharge standard, isolated gas phase, liquid phase, solid phase can directly drain in the environment after oily sludge was handled.
Embodiment 2
The grand celebration refinery contains the flotation cell scum silica frost of big water gaging, and water content is 80.6%, and oleaginousness is 15.9%, contains solids 3.5%, directly sends into the supercritical water oxidation still, and amount of water is 60mL, and reaction pressure is 26MPa, and temperature of reaction is 460 ℃, H
2O
2Make oxygenant, the oxygenant consumption is 5 times of theory demands amount, and the reaction times is 5 minutes.Handle back gas phase composition: O
2Be 21.6%, N
2Be 22.8%, CO
2Be 54.4%, CO is 1.2%.Handling back liquid COD is 42mg/L, and the pH value is 4.8, and solid phase is neither moisture, also oil-containing not.
The grand celebration oily sludge in slurry tank of four factories that recovers the oil, former water content is 36.8%, oleaginousness is 44.4%, solids content is 18.8%, through after pre-treatment extracts most of oil ingredient, oil-containing is 3.4%, water ratio 73.4%, and solids content is 23.2%.Oily sludge after handling is sent into the supercritical water oxidation still, and amount of water is 55mL, and reaction pressure is 30MPa, and temperature of reaction is 480 ℃, H
2O
2Make oxygenant, the oxygenant consumption is 4 times of theory demands amount, and the reaction times is 10 minutes.Handle back gas phase composition: O
2Be 20.6%, N
2Be 16.9%, CO
2Be 62.4%, CO is 0.1%.Handling back liquid COD is 26mg/L, and the pH value is 6.4, and solid phase is neither moisture, also oil-containing not.
Grand celebration oil extraction No.1 Factory crude oil storage tank oily sludge, oleaginousness 83.5%, water content 12.8%, containing solids is 3.7%, directly sends into the supercritical water oxidation still, and amount of water is 110mL, and reaction pressure is 24MPa, and temperature of reaction is 400 ℃, O
3Make oxygenant, the oxygenant consumption is 4 times of theory demands amount, and the reaction times is 8 minutes, handles back gas phase composition: O
2Be 44.8%, N
2Be 12.4%, CO
2Be 42.4%, CO is 0.4%; Handling back liquid COD is 48mg/L, and the pH value is 4.4, and solid phase is neither moisture, also oil-containing not.
The grand celebration oily sludge in slurry tank of seven factories that recovers the oil, oil-containing 30.4%, moisture 61.5%, contain solids 8.1%, directly send into the supercritical water oxidation still, amount of water is 135mL, and reaction pressure is 30MPa, and temperature of reaction is 380 ℃, air is made oxygenant, the oxygenant consumption is 3 times of theory demands amount, and the reaction times is 15 minutes, handles back gas phase composition: O
2Be 10.2%, N
2Be 77.6%, CO
2Be 11.9%, CO is 0.3%; Handling back liquid COD is 44mg/L, and the pH value is 4.6, and solid phase is oil-containing, also not moisture neither.
The grand celebration oily sludge in six factory's secondary settlement jars that recovers the oil, oil-containing 42.3%, moisture 55.5%, contain solids 2.2%, directly send into the supercritical water gasification reactor, amount of water is 50mL, and reaction pressure is 23MPa, and temperature of reaction is 500 ℃, hydrogen peroxide is made oxygenant, the oxygenant consumption is 5 times of theory demands amount, and the reaction times is 0.5 minute, handles back gas phase composition: O
2Be 38.2%, N
2Be 18.6%, CO
2Be 42.7%, CO is 0.5%; Handling back liquid COD is 44mg/L, and the pH value is 4.6, and solid phase is oil-containing, also not moisture neither.
The grand celebration oily sludge in eight factory's crude oil basins that recovers the oil, oil-containing 87.5%, moisture 11.2%, contain solids 1.3%, directly send into the supercritical water gasification reactor, amount of water is 100mL, and reaction pressure is 23MPa, and temperature of reaction is 420 ℃, hydrogen peroxide is made oxygenant, the oxygenant consumption is 5 times of theory demands amount, and the reaction times is 3 minutes, handles back gas phase composition: O
2Be 21.1%, N
2Be 15.7%, CO
2Be 62.8%, CO is 0.4%; Handling back liquid COD is 38mg/L, and the pH value is 5.4, and solid phase is oil-containing, also not moisture neither.
The grand celebration oily sludge in five factory's secondary settlement jars that recovers the oil, oil-containing 33.8%, moisture 63.5%, contain solids 2.7%, directly send into the supercritical water gasification reactor, amount of water is 95mL, and reaction pressure is 23MPa, and temperature of reaction is 440 ℃, hydrogen peroxide is made oxygenant, the oxygenant consumption is 3 times of theory demands amount, and the reaction times is 12 minutes, handles back gas phase composition: O
2Be 18.6%, N
2Be 10.4%, CO
2Be 70.8%, CO is 0.2%; Handling back liquid COD is 26mg/L, and the pH value is 5.8, and solid phase is oil-containing, also not moisture neither.
Claims (6)
1, a kind of method of utilizing supercritical water oxidation technical finesse oily sludge, concrete steps are as follows:
(1) a certain amount of oily sludge is put into reactor, and in reactor, add a certain amount of water;
(2) temperature and the pressure of setting reactor, wherein temperature is: 350 ℃～550 ℃, pressure is the emergent pressure of water: 22MPa～30MPa;
(3) inject oxygenant after heating reaches temperature of reaction;
(4) reaction 0.5min～15min;
(5) the laggard capable gas, liquid, solid three phase separation of reaction.
2, according to the described method of utilizing supercritical water oxidation technical finesse oily sludge of claim 1, it is characterized in that: the described amount that adds entry is calculated according to Martin-time equation.
3, according to the described method of utilizing supercritical water oxidation technical finesse oily sludge of claim 1, it is characterized in that: described temperature of reaction is 380 ℃～500 ℃.
4, according to the described method of utilizing supercritical water oxidation technical finesse oily sludge of claim 1, it is characterized in that: described oxygenant is oxygen (O
2), air, hydrogen peroxide (H
2O
2) or ozone (O
3) in a kind of.
5, according to the described method of utilizing supercritical water oxidation technical finesse oily sludge of claim 1, it is characterized in that: the amount of described oxygenant is 1～10 times of theoretical oxygen demand.
6, according to the described method of utilizing supercritical water oxidation technical finesse oily sludge of claim 5, it is characterized in that: the amount of described oxygenant is 3～6 times of theoretical oxygen demand.
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