CN105925300B - A kind of CO for oil-based drill cuttings treatment2The recovery method of switching mode solvent - Google Patents
A kind of CO for oil-based drill cuttings treatment2The recovery method of switching mode solvent Download PDFInfo
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- CN105925300B CN105925300B CN201610309010.2A CN201610309010A CN105925300B CN 105925300 B CN105925300 B CN 105925300B CN 201610309010 A CN201610309010 A CN 201610309010A CN 105925300 B CN105925300 B CN 105925300B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
- C10G1/045—Separation of insoluble materials
Abstract
The invention discloses a kind of CO for oil-based drill cuttings treatment2The recovery method of switching mode solvent, it is containing CO2Solid sodium hydroxide is first added in the water phase of switching mode solvent, upper oil phase and lower floor's water phase are isolated after stirring and dissolving；Solid oxidation calcium is added from the water phase isolated again, upper oil phase, mid-water phase and lower floor's solid phase are isolated after stirring and dissolving；Isolated oil phase is the CO of recovery2Switching mode solvent.The time required to the inventive method greatly shortens solvent recovery, solvent recovery efficiency is effectively increased, while the water quality of the waste water isolated also is improved very well, can be used as the pretreatment of organic amine waste water.
Description
Technical field
The present invention relates to a kind of recovery method of solvent, and in particular to a kind of CO for oil-based drill cuttings treatment2Switching mode
The recovery method of solvent, belongs to petrochemical industry oil-containing hazardous waste processing technology field high.
Background technology
With continuing to increase for the unconventional energy resource such as global shale gas, tight gas exploitation dynamics, oil base drilling fluid technology is
Through one of key technology as shale gas horizontal drilling.However, oil can be produced in Exploration of Oil And Gas, exploitation drilling process
The accumulation of base drilling cuttings.Because oil-based drill cuttings contain the pollutants such as petroleum hydrocarbon, heavy metal and organic matter, National Hazard has been put into it and has given up
Gurry (National Hazard waste register, HW08).
If oil-based drill cuttings are just directly discharged without treatment, it will cause serious harm to periphery ecological environment：Contained has
Machine thing will polluted surface water and groundwater resources, be mainly reflected in water-quality CODCrThe rising of value, the rising of colourity；Destruction soil
Earth, unfavorable to plant growth, serious caused soil cannot return cultivated；The poisonous and harmful substances such as heavy metal are detained soil, influence
The growth and the breeding of microorganism of plant, human body is entered by the effect of food chain, is detrimental to health.
Environmental protection is always the heavier problem for regarding of the mankind, is also the problem for meriting attention that country strongly calls, because
This solves the problems, such as that oil-based drill cuttings pollution environment is extremely urgent.At present for the treatment of oil-based drill cuttings, generally adopt both at home and abroad
Method has burning method, underground re-injection method, burial method, solidification method, heat treating process, solvent extraction, centrifugal separation etc..
CO2Switching mode solvent refers to toward being passed through in system and discharge CO2When, solvent physicochemical property (such as polarity, viscosity, molten
Solution property etc.) can phase co-conversion a kind of solvent, it can in a mild condition realize polarity and water miscible notable reversible change, by
There is the characteristic of intelligent switch in such solvent, without having too high requirement, low for equipment requirements, flow to temperature, pressure
With it is easy to operate, oil-based drill cuttings treatment application and promote on have well application and promotion potential.
CO2Switching mode solvent be used for oil-based drill cuttings processing method be：By the CO of equivalent2Switching mode solvent and oil-based drill cuttings
Mixing stirring at normal temperature 30min or so, CO2Switching mode solvent fully reacts with oil-based drill cuttings, and separation and Extraction goes out from oil-based drill cuttings
Mineral waste oils, is then centrifuged for isolating residue and mixing oils extract solution, to gauge water is added in extract solution, leads to CO2, in CO2
Stimulation induction under, the CO in extract solution2Switching mode solvent starts progressively to go in water phase, and after conversion is finished, upper oil phase is only
Mineral waste oils in remaining drilling cuttings, now can be separated and reclaims out oil phase, and remaining water is being passed through N2Or air discharge CO2Afterwards
It is capable of achieving CO2The recovery of switching mode solvent.But when solvent is separated and recovered, oil-based drill cuttings additive such as emulsifying agent, fluid loss additive pair
Water-borne glue body has protective effect, if being simply passed through N2Or the physical method such as air, heating is difficult to fast and effectively realize solvent
Separation.
The content of the invention
In view of this, it is an object of the invention to be directed to above-mentioned the deficiencies in the prior art, there is provided one kind efficiently can be returned quickly
Receive the CO for oil-based drill cuttings treatment2The method of switching mode solvent, saves reaction time, reducing energy consumption.
Be solve above technical problem, the technical solution adopted by the present invention provide it is a kind of for oil-based drill cuttings treatment
CO2The recovery method of switching mode solvent, it is comprised the following steps：
(1) containing CO2Solid sodium hydroxide is added in the water phase of switching mode solvent, natural layering is placed after stirring and dissolving,
Gravity Separation goes out upper oil phase and lower floor's water phase；
(2) in the water phase that step (1) is isolated add solid oxidation calcium, isolated after stirring and dissolving upper oil phase, in
Layer water phase and lower floor's solid phase；
(3) upper oil phase that the upper oil phase and step (2) that step (1) is separate are separate is the CO of recovery2Switching mode is molten
Agent.
It is described containing CO2The water of switching mode solvent refers to mutually to use CO2Isolated water after switching mode solvent treatment oil-based drill cuttings
Phase.Specially：By etc. quality oil-based drill cuttings and CO2Switching mode solvent mixes, and 30min is stirred under normal temperature, and centrifugation goes out residual
Slag and mixing oils extract solution, extract solution in mass ratio: water=1: 2 toward quantitative water is added in extract solution, under high velocity agitation
It is passed through CO2, after the 1h that ventilates under the 1L/min flux, isolated mineral oils and containing CO2The water phase of switching mode solvent.
Further, the addition present invention defines NaOH in step (1) is containing CO2The water phase of switching mode solvent
The 5~10% of weight.
Further, the addition present invention defines calcium oxide in step (2) is containing CO2The water of switching mode solvent is mutually overlapped
The 5~10% of amount.
Further, the stir speed (S.S.) present invention defines step (1) NaOH is 30r/min；Oxidation in step (2)
The stir speed (S.S.) of calcium is 30r/min.
Further, the separation method present invention defines step (1) is Gravity Separation, and the separation method of step (2) is
Centrifugation and Gravity Separation, and it is 4000r/min to further define the centrifugation rate of centrifugation, centrifugation time is
5min.Step (1) is first containing CO2Add solid sodium hydroxide in the water phase of switching mode solvent, the CO in NaOH and water phase2
Reaction, due to CO2Continuous reduction, solvent gradually separates from water phase, the proportion according to the two it is different by place from
So layering quickly Gravity Separation can go out solvent；Step (2) adds calcium oxide, calcium oxide and remaining CO in water phase2Reaction
Generate substantial amounts of CaCO3Sediment, suspension (including a small amount of solvent) forms floccule in adsorbing a large amount of water, therefore it is first passed through
Lower floor's solid phase (i.e. floccule) is isolated in centrifugation, then goes out upper oil phase (CO by placing natural layering Gravity Separation again2
Switching mode solvent) and mid-water phase (through the waste water after water quality adjustment), separating effect is more superior.
Further, the recovery method that the present invention is provided is particularly suited for CO2Switching mode solvent N, N- dimethyl cyclohexyl amine
Recovery.The effect that N, N- dimethyl cyclohexyl amine treatment oil-based drill cuttings reclaim waste mineral oil is good, and is reclaimed with the inventive method
The organic efficiency of N, N- dimethyl cyclohexyl amine is high.
With existing conventional logical N2Or air heating recovery CO2The method for switching solvent is compared, and the present invention has following excellent
Point：
(1) present invention greatly shortens solvent recovery required time by adding chemical reagent, effectively increases solvent
Organic efficiency, solvent recovery efficiency is up to 92%；
(2) gas need not be passed through during present invention reaction, due to NaOH and CaO when be dissolved in water meeting lower to equipment requirement
Generation hydrated ion, releases amount of heat, so as to reduce CO2Solubility of the gas in water, therefore without hyperthermic treatment,
Management cost is lower；
(3) when the present invention adds CaO, hydrated ion is generated with water, can effectively destroys water-borne glue body double electrical layerses, so that
Make elimination of colloid stability, while forming substantial amounts of CaCO3Sediment, adsorbs suspension (including a small amount of solvent) in a large amount of water, forms wadding
Shape thing, so as to get water phase in ammonia-nitrogen content (NH3- N), biodegradability (B/C), COD (COD), suspension content
Etc. (SS) water quality index is improved very well, can be used as the pretreatment of organic amine waste water.
Specific embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to specific embodiment pair
The present invention is described in further detail.It should be pointed out that following preferred embodiments are not construed as limitation of the present invention,
Protection scope of the present invention should be defined by claim limited range.Come for those skilled in the art
Say, without departing from the spirit and scope of the present invention, can also make some improvements and modifications, these improvements and modifications should also be regarded
It is protection scope of the present invention.
Step one, with containing CO2Switching mode solvent processes oil-based drill cuttings
Take 100g oil-based drill cuttings and 100gCO2Switching mode solvent N, N- dimethyl cyclohexyl amine (CyNMe2) mixing, stirred under normal temperature
Mix 30min, centrifugation goes out residue 82g and mixing oils extract solution 118g, in mass ratio extract solution: water=1: 2 toward extract solution
It is middle to add quantitative water, CO is passed through under high velocity agitation2, after the 1h that ventilates under the 1L/min flux, isolated mineral oils and
Containing CO2The water phase 336g of switching mode solvent.
Step 2, containing CO2The water analysis of the water phase of switching mode solvent
By step one obtain containing CO2The water of switching mode solvent mutually carries out water analysis, with reference to water standard《The Chinese people
Republic's integrated wastewater discharge standard》(GB 8978-1996).
NH3The measure normative reference of-N (ammonia-nitrogen content)《The measure (reagent colorimetric method) of ammonia nitrogen in water》(HJ535-
2009) NH, is determined using Na's reagent3-N；The measure normative reference of COD (COD)《Water chemical oxygen demand
Determine dichromic acid sylvite method》(GB11914-89) COD, is determined using dichromate titration；The measure normative reference of BOD5《Water quality five
The measure dilution of day biochemical oxygen demand (BOD) (BOD5) and inocalation method》(HJ 505-2009), BOD5 is determined using oxygen demand on the five；
The measure of biodegradability B/C is using BOD5 (biochemical oxygen demand (BOD) on the 5th) and COD ratios；Using ss suspended solid in gravimetric detemination water,
Using the colourity of dilution-colorimetric method for determining water.Water analysis is shown in Table 1.
Step 3, from containing CO2CyNMe is reclaimed in the water phase of switching mode solvent2
Take that step one obtains containing CO2The water phase 336g of switching mode solvent is equally divided into 8 parts, every part of 42g, respectively with following
The method of embodiment is reclaimed：
Embodiment 1：Take a containing CO2The water phase 42g of switching mode solvent, adds solid sodium hydroxide 2.1g, stirring and dissolving
Isolated upper oil phase 6.25g and lower floor's water phase, water analysis is mutually carried out to lower floor's water afterwards, is specifically shown in Table 1.
Embodiment 2：Take a containing CO2The water phase 42g of switching mode solvent, adds solid sodium hydroxide 4.2g, stirring and dissolving
Isolated upper oil phase 8.75g and lower floor's water phase, water analysis is mutually carried out to lower floor's water afterwards, is specifically shown in Table 1.
Embodiment 3：Take a containing CO2The water phase 42g of switching mode solvent, adds solid oxidation calcium 2.1g, after stirring and dissolving
Isolated upper oil phase 4.38g, mid-water phase and lower floor's solid phase, water analysis is mutually carried out to mid-water, is specifically shown in Table 1.
Embodiment 4：Take a containing CO2The water phase 42g of switching mode solvent, adds solid oxidation calcium 4.2g, after stirring and dissolving
Isolated upper oil phase 5g, mid-water phase and lower floor's solid phase, water analysis is mutually carried out to mid-water, is specifically shown in Table 1.
Embodiment 5：Take a containing CO2The water phase 42g of switching mode solvent, adds solid sodium hydroxide 2.1g, stirring and dissolving
Isolated upper oil phase 6.25g and lower floor's water phase, then to solid oxidation calcium 4.2g is added in separate lower floor's water phase, stir afterwards
Mix separated and dissolved and obtain upper oil phase 3.75g, mid-water phase and lower floor's solid phase, water analysis is mutually carried out to mid-water, be specifically shown in
Table 1.
Embodiment 6：Take a containing CO2The water phase 42g of switching mode solvent, adds solid sodium hydroxide 4.2g, stirring and dissolving
Isolated upper oil phase 8.75g and lower floor's water phase afterwards, then to adding solid oxidation calcium 4.2g in separate lower floor's water phase,
The isolated upper oil phase 2.75g of stirring and dissolving, mid-water phase and lower floor's solid phase, mutually carry out water analysis, specifically to mid-water
It is shown in Table 1.
Embodiment 7：Take a containing CO2The water phase 42g of switching mode solvent, is passed through N under high velocity agitation2, in 1L/min flux
After lower ventilation 1h, isolated upper oil phase 4.96g and lower floor's water phase mutually carry out water analysis to lower floor's water, are specifically shown in Table 1.
Embodiment 8：Take a containing CO2The water phase 42g of switching mode solvent, is passed through N under high velocity agitation2, in the condition of heating
Under with 1L/min flux ventilation 1h after, isolated upper oil phase 5.63g and lower floor's water phase mutually carry out water quality point to lower floor's water
Analysis, is specifically shown in Table 1.
Step 4, data analysis
4.1 water quality index are analyzed
The water quality index analytical table of table 1.
| Project | SS(g/ml) | Colourity | COD(mg/L) | B/C | |
| Before recovery | 247 | 256 | 300 | 4700 | 0.1 |
| Embodiment 1 | 226 | 230 | 280 | 3200 | 0.2 |
| Embodiment 2 | 224 | 228 | 270 | 3200 | 0.2 |
| Embodiment 3 | 60 | 20 | 105 | 2600 | 0.3 |
| Embodiment 4 | 56 | 16 | 100 | 2400 | 0.3 |
| Embodiment 5 | 58 | 18 | 110 | 2400 | 0.3 |
| Embodiment 6 | 56 | 16 | 100 | 2400 | 0.3 |
| Embodiment 7 | 238 | 255 | 280 | 4600 | 0.1 |
| Embodiment 8 | 238 | 255 | 285 | 4650 | 0.1 |
As can be seen from the above table, CO is reclaimed with the inventive method2Switching mode solvent, the ammonia in the waste water obtained after treatment
Nitrogen content (NH3- N), biodegradability (B/C), COD (COD), the water quality index such as suspension content (SS) is obtained very well
Improve, can be used as the pretreatment of organic amine waste water；With conventional logical N2The method of recycling design and the only recovery of hydrogenation sodium oxide molybdena are molten
The method of agent, water quality is not all significantly improved.
4.2 organic efficiencies are analyzed
Used by embodiment 1-8 containing CO2The water of switching mode solvent is mutually the step of respectively one water phase, in step one
CyNMe2Addition be 100g, so CyNMe in each embodiment2Addition be 100/8=12.5g.
The solvent recovery efficiency of table 2.
As can be seen from the above table, with existing conventional logical N2Recuperation of heat CO2The method for switching solvent is compared, and the present invention is returned
Receive solvent method greatly shorten solvent recovery needed for time, solvent recovery efficiency also effectively improved, and solvent is returned
Rate produce effects up to 92%.
Claims (8)
1. it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, it is characterised in that：Comprise the following steps：
(1) containing CO2Add solid sodium hydroxide in the water phase of switching mode solvent, isolated after stirring and dissolving upper oil phase and under
Layer water phase；
(2) solid oxidation calcium is added in the water phase that step (1) is isolated, upper oil phase, mid-water is isolated after stirring and dissolving
Mutually with lower floor's solid phase；
(3) upper oil phase that the upper oil phase and step (2) that step (1) is separate are separate is the CO of recovery2Switching mode solvent；
It is described containing CO2The water of switching mode solvent refers to mutually to use CO2Isolated water phase after switching mode solvent treatment oil-based drill cuttings.
2. it is according to claim 1 it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, its feature
It is：The addition of NaOH is containing CO in the step (1)2The 5~10% of the water phase weight of switching mode solvent.
3. it is according to claim 1 it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, its feature
It is：The addition of calcium oxide is containing CO in the step (2)2The 5~10% of the water phase weight of switching mode solvent.
4. it is according to claim 1 it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, its feature
It is：The stir speed (S.S.) of NaOH is 30r/min in the step (1).
5. it is according to claim 1 it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, its feature
It is：The speed of the stirring and dissolving of calcium oxide is 30r/min in the step (2).
6. it is according to claim 1 it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, its feature
It is：The separation method of the step (1) is Gravity Separation, and the separation method of step (2) is centrifugation and Gravity Separation.
7. it is according to claim 6 it is a kind of for oil-based drill cuttings treatment CO2The recovery method of switching mode solvent, its feature
It is：The centrifugation rate of the centrifugation is 4000r/min, and centrifugation time is 5min.
8. it is according to any one of claim 1 to 7 it is a kind of for oil-based drill cuttings treatment CO2The recovery of switching mode solvent
Method, it is characterised in that：The CO2Switching mode solvent is N, N- dimethyl cyclohexyl amines.
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| CN106902551A (en) * | 2017-03-31 | 2017-06-30 | 昆明理工大学 | A kind of breaking method of emulsion |
| CN107376421A (en) * | 2017-09-11 | 2017-11-24 | 扬州大学 | A kind of method for carrying out extract and separate to the blend of organic matter and water using N methyl diethanolamines |
| CN108862954B (en) * | 2018-06-29 | 2021-05-28 | 西南石油大学 | Method for treating oily waste by adopting switch type mixed solvent system |
| CN111298734B (en) * | 2020-02-22 | 2021-11-30 | 西南石油大学 | NaHSO3Preparation method of ethyl cellulose microcapsule |
| CN114425180B (en) * | 2020-10-10 | 2023-08-08 | 中国石油化工股份有限公司 | Improved eutectic solvent, preparation method thereof and application of improved eutectic solvent in separation of polycyclic aromatic hydrocarbon |
| CN112391190B (en) * | 2020-11-17 | 2022-02-25 | 西南石油大学 | CO2/N2 switch type double-circulation extraction process and application thereof |
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| CN105154124A (en) * | 2015-10-10 | 2015-12-16 | 山东大学 | Method for treating oily cuttings by adopting switch-type solvent |
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| US10363336B2 (en) * | 2011-08-26 | 2019-07-30 | Battelle Energy Alliance, Llc | Methods and systems for treating liquids using switchable solvents |
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| CN104804759A (en) * | 2015-03-17 | 2015-07-29 | 西南石油大学 | Oil-based drilling cutting treatment method |
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