CN106010623A - Extracting solvent for treating oil-based drillings and preparation method thereof - Google Patents
Extracting solvent for treating oil-based drillings and preparation method thereof Download PDFInfo
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- CN106010623A CN106010623A CN201610604872.8A CN201610604872A CN106010623A CN 106010623 A CN106010623 A CN 106010623A CN 201610604872 A CN201610604872 A CN 201610604872A CN 106010623 A CN106010623 A CN 106010623A
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- extractant
- oil
- solvent
- drill cuttings
- based drill
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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
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
Abstract
The invention belongs to the technical field of oil-based drilling treatment, and particularly relates to an extracting solvent for treating oil-based drillings and a preparation method thereof. The extracting solvent is prepared from alkyl chloride, magnesium powder and vinyl chloride in a solvent. The preparation method comprises the following steps: adding the solvent in a reaction vessel, pumping nitrogen for protection, and then sequentially adding the solvent, the alkyl chloride and the magnesium powder for reaction; then adding a catalyst and the vinyl chloride in the reaction vessel for reaction, and heating, distilling and filtering after the reaction is completed, thus obtaining the extracting solvent. According to the extracting solvent disclosed by the invention, the problems of lower circulation utilization rate, higher economic cost, serious environment pollution and serious potential safety hazard caused by volatility and low flash point of an existing conventional solvent are solved, and the extracting solvent has the advantages of high flash point, high security, good extracting effect, high recovery rate, small emission pollution, simple process technology, easiness in implementation and the like.
Description
Technical field
The invention belongs to oil-based drill cuttings processing technology field, be specifically related to a kind of process oil-based drill cuttings extractant and
Preparation method.
Background technology
In drilling process, oil base drilling fluid has irreplaceable advantage compared with water-base drilling fluid, and its technology, technique also compare
Ripe.Therefore use oil base drilling fluid drilling well to get more and more, be widely used to shale gas and the deep-well of normal gas pools, ultra-deep
Well, horizontal well, prospect pit etc. are drilled well.But the oil-based drill cuttings produced in drilling process is oil-containing danger wastes, to environment, ecology
And safety all produces serious influence.
After mainly using pyrolysis, eccentric part removing oil for this type of oil-based drill cuttings at present, packing is sent outside and Conventional solvents extraction
Technology processes, and above-mentioned processing method exists energy consumption height, potential safety hazard is big, process thorough, high in cost of production problem.Oil simultaneously
The general oil content of base drilling cuttings, between 15-20%, itself has the highest recycle value.Implement along with new environmental law and environment is protected
Protect, the reinforcement of security control, solve that oil-gas mining oil-based drill cuttings is innoxious, recycling problem becomes oil and gas industry environment and protects
Protect, keep the safety in production new problem and urgent need to solve the problem.
During processing oil-based drill cuttings, solvent extraction technology is crucial technology, and wherein, extractant is solvent extraction skill
The core of art, and conventional at present extractant mainly low-carbon (LC) alcohols, petroleum ether or chloroform, dichloromethane etc. are easily waved
Send out, flash-point is low or toxicity is stronger organic solvent.This kind of extractants displacement efficiency is higher, but recovery utilization rate is relatively low, exists into
The problems such as this height, security risk are big, operation easier is big.It is therefore desirable to develop a kind of novel extractant, meet oil gas field
" safe and environment-friendly, efficient, harmonious " sustainable exploration and development needs.
Summary of the invention
It is an object of the invention to overcome that the existing Conventional solvents of existing solution is volatile and flash-point is low, cause cyclic utilization rate relatively
Low, Financial cost is the highest, there is serious environmental pollution and security hidden trouble.
To this end, the invention provides a kind of process oil-based drill cuttings extractant, by the following raw material by quality proportioning
Incorporate solvent to be prepared from:
Chloralkane, 40~60 parts;
Magnesium dust, 5~10 parts;
Chloroalkene, 20~40 parts,
Described solvent quality is the 40~60% of raw material gross mass.
Described chloralkane is 1-chlorododecane or 1-chlorine tridecane or the 1-chlorine tetradecane.
Described magnesium dust particle diameter is in 75 μm~150 μm, and its purity is more than 99.5%.
Described chloroalkene is tetrachloroethylene or trichloro ethylene.
Described solvent is absolute ether or oxolane.
A kind of preparation method processing oil-based drill cuttings extractant, comprises the steps:
1), raw material is weighed respectively according to proportional quantity: chloralkane, magnesium dust and chloroalkene;And prepare raw material gross mass
40~the solvent of 60%;
2), it is sequentially added into solvent, chloralkane and magnesium dust that step 1) prepares, when reaction temperature reaches 20~30 DEG C, with
100r/min rotating speed stirring reaction 1~3h;
3), in reaction vessel, catalyst and the chloroalkene of step 1) preparation are added, when reaction temperature reaches 50~70 DEG C, with
100r/min rotating speed stirring reaction 3~6h;
4), reacted after, be heated to 70~80 DEG C of distillations and filter, preparing required process oil-based drill cuttings and extract molten
Agent.
Described step 2) in, before adding solvent and raw material, in reaction vessel, it is passed through nitrogen protects.
The described catalyst in step 3) is Cu-lyt., and its quality is in step 1) the 1% of raw material gross mass.
The beneficial effect of this process oil-based drill cuttings extractant that the present invention provides:
(1) compared with Conventional solvents, this extractant has higher flash-point, and in practical operation, safety is high;
(2) this extractant and diesel oil, white oil, gas liquefaction intermiscibility are good, can be used for processing the oil-based drill cuttings containing different base oils;
(3) this extractant is in oil-based drill cuttings surface adsorption ability, and beneficially extractant reclaims and separates, and does not bring secondary
Pollute;
(4) this extractant effect of extracting is good, and the oil-based drill cuttings oil content after process is less than 1%;
(5) this recovery rate of extraction solvent is up to more than 95%, and the extractant of recovery can realize recycled for multiple times;
(6) this extractant and base oil good separating effect, the base oil of recovery can be used for preparing oil base drilling fluid;
(7), after oil-based drill cuttings is processed by this extractant, residue leachate and heavy metal reach country's integrated wastewater discharge
The first discharge standard of standard " GB8978 2002 ";
(8) this extractant processes oil-based drill cuttings technological process simply, low for equipment requirements, it is easy to implement.
Detailed description of the invention
Embodiment 1:
The present embodiment one process oil-based drill cuttings extractant, by following by the raw material of quality proportioning incorporate solvent preparation and
Become:
The chloralkane of 40~60 parts, chloralkane is 1-chlorododecane or 1-chlorine tridecane or the 1-chlorine tetradecane;
The magnesium dust of 5~10 parts, magnesium dust particle diameter is in 75 μm~150 μm;
The chloroalkene of 20~40 parts, chloroalkene is tetrachloroethylene or trichloro ethylene;
Wherein, solvent quality is the 40~60% of raw material gross mass, and solvent is absolute ether or oxolane.
The present embodiment provide a kind of oil-soluble is good, volatility is low and the extractant of high-flash, can solve existing often
Rule solvent is volatile and flash-point is low, causes cyclic utilization rate relatively low, and Financial cost is the highest, there is serious environmental pollution and peace
Full potential problem.
Embodiment 2:
The present embodiment provides a kind of preparation method processing oil-based drill cuttings extractant, comprises the steps:
1), raw material is weighed respectively according to proportional quantity: chloralkane, magnesium dust and chloroalkene;And prepare raw material gross mass
40~the solvent of 60%;
2), in reaction vessel, it is passed through nitrogen protects, be then sequentially added into solvent, chloralkane and magnesium that step 1) prepares
Powder, when reaction temperature reaches 20~30 DEG C, with 100r/min rotating speed stirring reaction 1~3h;
3), in reaction vessel, add the chloroalkene that catalyst Cu-lyt. and step 1) prepare, reaction temperature reach 50~
When 70 DEG C, with 100r/min rotating speed stirring reaction 3~6h;
4), reacted after, be heated to 70~80 DEG C of distillations and filter, preparing required process oil-based drill cuttings and extract molten
Agent.
Embodiment 3:
The present embodiment in conjunction with the embodiments 1 and embodiment 2 carry out being embodied as explanation:
The present embodiment provides one to process oil-based drill cuttings extractant, following be prepared from by the raw material of quality proportioning:
The 1-chlorine tetradecane: 60 parts, particle diameter 75 μm magnesium dust (purity 99.8%): 5 parts, tetrachloroethylene: 35 parts.
This process oil-based drill cuttings extractant is prepared in accordance with the following methods: weigh raw material respectively according to proportioning, point
Another name takes absolute ether and 1% Cu-lyt. of quality is raw material gross mass 50%;In reaction vessel, it is passed through nitrogen carry out
Protection, is proportionally added into absolute ether, the 1-chlorine tetradecane, magnesium dust successively, keeps 20 DEG C of stirring at 100r/min rotating speed of temperature
Mix lower reaction 2h;It is sequentially added into Cu-lyt., tetrachloroethylene, stirring of 100r/min rotating speed, simultaneously by reaction vessel
It is heated to 60 DEG C of stirring 5h;Continuing to be heated to 75 DEG C and distill out absolute ether, filtering solution removes solid phase, prepares present treatment oil base
Drilling cuttings extractant.
The performance test processing oil-based drill cuttings extractant that the present embodiment provides is as follows:
Test 1: extractant flashing test.
Survey by the test method of national standard " flashing test Bin Siji-Martin remain silent agar diffusion method " (GB-T 261-2008)
Determining the flash-point of extractant, the flash-point recording extractant is 47 DEG C.Compared to the flammable liquid flash-point less than 45 DEG C, this extraction
Solvent has higher flash-point, and in practical operation, safety is high.
Test 2: extractant effect of extracting is evaluated.
Take quantitative oil-based drill cuttings, add the extractant of 2 times of quality, stirring at normal temperature 15min, go out residue through centrifugation
And liquid phase, residue to be separated out uses state environment protecting standard " water quality through heating recovery solvent, the residue after drying
The mensuration infrared spectrophotometer of petroleum class and zoology and botany oil class " the determination of test method oil content of (HJ 637-2012), contain
Oil rate is shown in Table 1.
Residue oil content after table 1 extraction
As seen from the above table, this extractant and diesel oil, white oil, gas liquefaction intermiscibility are good, can be used for processing containing different base oils
Oil-based drill cuttings.
Test 3: recovery rate of extraction solvent.
Liquid phase after centrifugation, according to extractant and the difference of base oil boiling point, the method using distillation, to extraction
Solvent reclaims, and the response rate is shown in Table 2.
Test 4: the effect of extracting that extractant repeatedly recycles and reuses
For same extractant, when extraction, distillation are repeated several times, the effect of extracting of oil-based drill cuttings is shown in Table by extractant
2。
Table 2 residue oil content and solvent recovering rate
As shown in Table 2, this extractant is in oil-based drill cuttings surface adsorption ability, and beneficially extractant reclaims and separates, no
Bring secondary pollution;This extractant effect of extracting is good, and the oil-based drill cuttings oil content after process is less than 1%;This extractant reclaims
Rate is up to more than 95%, and the extractant of recovery can realize recycled for multiple times;This extractant and base oil good separating effect,
The base oil reclaimed can be used for preparing oil base drilling fluid.
Test 5: the flash-point Changing Pattern in extractant repeatedly extraction process
For same extractant, through extraction, distillation are repeated several times, measure its flash-point change feelings in different numbers of repetition
Condition, experimental result such as table 3.
The recycling of table 3 extractant changes with flash-point
Test 6: extractant processes the main contamination index of oil-based drill cuttings residue and analyzes
Using this extractant to process oil-based drill cuttings, the residue after process has carried out relevant environmental protection and has referred to test analysis, point
Analysis result such as table 4.
Residue analysis after table 4 oil-based drill cuttings extraction process
After oil-based drill cuttings is processed by this extractant, residue leachate and heavy metal reach national sewage comprehensive emission standard
The first discharge standard of " GB8978 2002 ".
Embodiment 4:
The present embodiment provides one to process oil-based drill cuttings extractant, following be prepared from by the raw material of quality proportioning:
1-chlorine tridecane: 55 parts, particle diameter 150 μm magnesium dust (purity 99.9%): 8 parts, trichloro ethylene: 37 parts.
This process oil-based drill cuttings extractant is prepared in accordance with the following methods: weigh raw material respectively according to proportioning, point
Another name takes oxolane and 1% Cu-lyt. of quality is raw material gross mass 60%;In reaction vessel, it is passed through nitrogen carry out
Protection, is proportionally added into oxolane, 1-chlorine tridecane, magnesium dust successively, keeps 25 DEG C of stirring at 100r/min rotating speed of temperature
Mix lower reaction 3h;It is sequentially added into Cu-lyt., trichloro ethylene, stirring of 100r/min rotating speed, simultaneously by reaction vessel
It is heated to 70 DEG C of stirring 5.5h;Continuing to be heated to 80 DEG C and distill out oxolane, filtering solution removes solid phase, prepares present treatment oil
Base drilling cuttings extractant.
With reference to the method for testing of embodiment 3, the extractant prepared by comparative example is tested, test result such as table
Shown in 5 to table 9.
Embodiment 5:
The present embodiment provides one to process oil-based drill cuttings extractant, following be prepared from by the raw material of quality proportioning:
1-chlorododecane: 54 parts, the pure magnesium dust of particle diameter 75 μm: 6 parts, tetrachloroethylene: 40 parts.
This process oil-based drill cuttings extractant is prepared in accordance with the following methods: weigh raw material respectively according to proportioning, point
Another name takes absolute ether and 1% Cu-lyt. of quality is raw material gross mass 55%;In reaction vessel, it is passed through nitrogen carry out
Protection, is proportionally added into absolute ether, 1-chlorododecane, magnesium dust successively, keeps 30 DEG C of stirring at 100r/min rotating speed of temperature
Mix lower reaction 3h;It is sequentially added into Cu-lyt., tetrachloroethylene, stirring of 100r/min rotating speed, simultaneously by reaction vessel
It is heated to 60 DEG C of stirring 5h;Continuing to be heated to 70 DEG C and distill out absolute ether, filtering solution removes solid phase, prepares present treatment oil base
Drilling cuttings extractant.
With reference to the method for testing of embodiment 3, the extractant prepared by comparative example is tested, test result such as table
Shown in 5 to table 9.
Embodiment 6:
The present embodiment provides one to process oil-based drill cuttings extractant, following be prepared from by the raw material of quality proportioning:
1-chlorododecane: 40 parts, the pure magnesium dust of particle diameter 100 μm: 10 parts, tetrachloroethylene: 30 parts.
This process oil-based drill cuttings extractant is prepared in accordance with the following methods: weigh raw material respectively according to proportioning, point
Another name takes absolute ether and 1% Cu-lyt. of quality is raw material gross mass 40%;In reaction vessel, it is passed through nitrogen carry out
Protection, is proportionally added into absolute ether, 1-chlorododecane, magnesium dust successively, keeps 25 DEG C of stirring at 100r/min rotating speed of temperature
Mix lower reaction 1.5h;It is sequentially added into Cu-lyt., tetrachloroethylene, stirring of 100r/min rotating speed, reaction is held simultaneously
Device is heated to 50 DEG C of stirring 4h;Continuing to be heated to 75 DEG C and distill out absolute ether, filtering solution removes solid phase, prepares present treatment oil
Base drilling cuttings extractant.
With reference to the method for testing of embodiment 3, the extractant prepared by comparative example is tested, test result such as table
Shown in 5 to table 9.
Embodiment 7:
The present embodiment provides one to process oil-based drill cuttings extractant, following be prepared from by the raw material of quality proportioning:
1-chlorododecane: 45 parts, particle diameter 110 μm magnesium dust (purity 99.7%): 7 parts, tetrachloroethylene: 20 parts.
This process oil-based drill cuttings extractant is prepared in accordance with the following methods: weigh raw material respectively according to proportioning, point
Another name takes absolute ether and 1% Cu-lyt. of quality is raw material gross mass 45%;In reaction vessel, it is passed through nitrogen carry out
Protection, is proportionally added into absolute ether, 1-chlorododecane, magnesium dust successively, keeps 28 DEG C of stirring at 100r/min rotating speed of temperature
Mix lower reaction 1h;It is sequentially added into Cu-lyt., tetrachloroethylene, stirring of 100r/min rotating speed, simultaneously by reaction vessel
It is heated to 55 DEG C of stirring 3h;Continuing to be heated to 75 DEG C and distill out absolute ether, filtering solution removes solid phase, prepares present treatment oil base
Drilling cuttings extractant.
With reference to the method for testing of embodiment 3, the extractant prepared by comparative example is tested, test result such as table
Shown in 5 to table 9.
Table 5: residue oil content contrast table after the extraction of each embodiment
Analyzed from table 5, the extractant prepared by each embodiment, relatively good with diesel oil, white oil, gas liquefaction intermiscibility,
Can be used for processing the oil-based drill cuttings containing different base oils.
Table 6: each embodiment residue oil content contrast table
Being analyzed from table 6, extractant prepared by each embodiment, in oil-based drill cuttings surface adsorption ability, is conducive to extracting molten
Agent is reclaimed and is separated, and does not bring secondary pollution;Each embodiment extractant effect of extracting is relatively good, the oil-based drill cuttings after process
Oil content is below 1%.
Table 7: each embodiment solvent recovering rate contrast table
Being analyzed from table 7, in each embodiment, the response rate of this extractant is up to more than 93%, and the extractant of recovery can be real
Existing recycled for multiple times;Extractant and base oil good separating effect, the base oil of recovery can be used for preparing oil base drilling fluid.
Table 8: the recycling of each embodiment extractant and flash-point change contrast table
Being analyzed from table 8, in each embodiment, the flash-point of the extractant of configuration is above 45 DEG C, therefore compared to inflammable liquid
The body flash-point less than 45 DEG C, extractant has higher flash-point, and in practical operation, safety is high.
Table 9: after each embodiment oil-based drill cuttings extraction processes, residue analysis contrasts table
Analyzed from table 9, in each embodiment, after oil-based drill cuttings is processed by the extractant of configuration, residue leachate and
Heavy metal all can reach the first discharge standard of national sewage comprehensive emission standard " GB8978 2002 ", meets constitutional law regulation
Discharge standard.
In sum, this process oil-based drill cuttings extractant that the present invention provides, compared with Conventional solvents, has relatively
High flash-point, in practical operation, safety is high;This extractant and diesel oil, white oil, gas liquefaction intermiscibility are good, can be used for processing
Oil-based drill cuttings containing different base oils;This extractant is in oil-based drill cuttings surface adsorption ability, and beneficially extractant reclaims
And separation, do not bring secondary pollution;This extractant effect of extracting is good, and the oil-based drill cuttings oil content after process is less than 1%;This extraction
Taking solvent recovering rate up to more than 95%, the extractant of recovery can realize recycled for multiple times;This extractant divides with base oil
From effective, the base oil of recovery can be used for preparing oil base drilling fluid;After oil-based drill cuttings is processed by this extractant, residue
Leachate and heavy metal reach the first discharge standard of national sewage comprehensive emission standard " GB8978 2002 ";This extractant
Process oil-based drill cuttings technological process simple, low for equipment requirements, it is easy to implement.
Exemplified as above is only the illustration to the present invention, is not intended that the restriction to protection scope of the present invention, all
It is within design same or analogous with the present invention belongs to protection scope of the present invention.
Claims (8)
1. one kind processes oil-based drill cuttings extractant, it is characterised in that: incorporated solvent by following by the raw material of quality proportioning
It is prepared from:
Chloralkane, 40~60 parts;
Magnesium dust, 5~10 parts;
Chloroalkene, 20~40 parts,
Described solvent quality is the 40~60% of raw material gross mass.
2. process oil-based drill cuttings extractant as claimed in claim 1, it is characterised in that: described chloralkane is 1-chlorine
Dodecane or 1-chlorine tridecane or the 1-chlorine tetradecane.
3. process oil-based drill cuttings extractant as claimed in claim 1, it is characterised in that: described magnesium dust particle diameter is 75
μm~150 μm, and its purity is more than 99.5%.
4. process oil-based drill cuttings extractant as claimed in claim 1, it is characterised in that: described chloroalkene is tetrachloro
Ethylene or trichloro ethylene.
5. process oil-based drill cuttings extractant as claimed in claim 1, it is characterised in that: described solvent is absolute ether
Or oxolane.
6. the preparation method processing oil-based drill cuttings extractant as described in any one in Claims 1 to 5, it is special
Levy and be, comprise the steps:
1), raw material is weighed respectively according to proportional quantity: chloralkane, magnesium dust and chloroalkene;And prepare raw material gross mass
40~the solvent of 60%;
2), it is sequentially added into solvent, chloralkane and magnesium dust that step 1) prepares, when reaction temperature reaches 20~30 DEG C, with
100r/min rotating speed stirring reaction 1~3h;
3), in reaction vessel, catalyst and the chloroalkene of step 1) preparation are added, when reaction temperature reaches 50~70 DEG C, with
100r/min rotating speed stirring reaction 3~6h;
4), reacted after, be heated to 70~80 DEG C of distillations and filter, preparing required process oil-based drill cuttings and extract molten
Agent.
7. the preparation method processing oil-based drill cuttings extractant as claimed in claim 6, it is characterised in that: described step
2), in, before adding solvent and raw material, in reaction vessel, it is passed through nitrogen protects.
8. the preparation method processing oil-based drill cuttings extractant as claimed in claim 6, it is characterised in that: described step
3) catalyst in is Cu-lyt., and its quality is in step 1) the 1% of raw material gross mass.
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