CN106010621A - Separating and recycling method and system for heavy oil deposit rich in carbonate - Google Patents
Separating and recycling method and system for heavy oil deposit rich in carbonate Download PDFInfo
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- CN106010621A CN106010621A CN201610298740.7A CN201610298740A CN106010621A CN 106010621 A CN106010621 A CN 106010621A CN 201610298740 A CN201610298740 A CN 201610298740A CN 106010621 A CN106010621 A CN 106010621A
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Classifications
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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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
-
- 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
-
- 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
Abstract
The invention relates to a separating and recycling method and system for heavy oil deposit rich in carbonate. Carbonate mineral substance containing heavy oil resources such as oil sand, oil shale and oily sludge are mixed with a prepared solution and a chemical additive for reacting under the certain condition, mineral substances in the heavy oil deposit are dissolved, and then the purpose of separating heavy oil from mineral particles is achieved; the separated heavy oil is subjected to subsequent processing treatment to further remove entrained water and solid particles, and a clean heavy oil product is obtained; waste liquid and mineral substance precipitates which are generated in the previous process are recycled separately, and then harmless discharge is finally achieved. Therefore, not only is the heavy oil extracted out from the oil deposit effectively, but also energy sources are greatly saved, and the energy-saving and emission-reducing production purposes of normal-temperature extracting or heavy oil recycling are achieved.
Description
Technical field
The present invention relates to a kind of from rich in carbonate heavy oil field is isolated the separation method of mink cell focus, belonging to
Work point from and reaction engineering technical field, be specifically related to crush, react, settle, filter, distill, crystallization etc.
Method.
Background technology
Heavy oil field (e.g., oil-sand, oil shale, landing oil, greasy filth etc.) be a kind of by mink cell focus (or Colophonium),
The grains of sand, clay and the complex mixture of a small amount of water composition.Because its process is huge, it is increasingly becoming a kind of standby
Petroleum resources.As a example by oil-sand, its proved reserves account for about 1/3rd of existing petroleum resources total amount, existing
Have technologically recoverable reserves to be about 651,000,000,000 barrels, be mainly distributed on Canada, Venezuela, the U.S., Russia,
The ground such as Indonesia and China, are a kind of very promising substitute energy source for petroleums.
The exploitation of oil-sand can be divided into strip mining transformation and in-situ extraction according to himself physicochemical property and geological conditions.
For Canadian moisturizing type oil-sand, when mineral products buried depth is less than 75 meters, industrial main employing thermokalite
Oil-sand is separated by washing process;And when oil-sand ore deposit buried depth is more than 75 meters, then use in-situ extraction
Method, as to bottom inject vapours, hot solvent etc..But, for glossy property oil-sand, such as the U.S. still
Oil-sand is dripped by the technique that his state oil-sand, Indonesia's oil-sand and Xinjiang, China oil-sand then cannot effectively utilize thermokalite to wash
Green grass or young crops separates.Other new techniques many to this end, be born, as solvent extraction technology (CN 101274303A,
CN 101544902A, CN102925190A, US 3117922 (1964), US 3392105 (1968),
US 4046669 (1969), US 4046668 (1977), US 4036732 (1977), US 4347118 (1982),
US 4498971 (1984), US 4929341 (1990)), pyrolysis technology (CN103289715A,
CN104087329A), microbial fermentation technology etc..These technology have respective advantage, such as, molten
Agent abstraction technique have extraction yield is high, extraction process need not water participation, can operate under room temperature, solvent can follow
The advantages such as ring use;Pyrolysis technology can realize mink cell focus extraction and refine oil integrated process, decreases technique mistake
Journey;What microbial fermentation technology can realize gentleness puies forward oil process etc..But, they are the most all along with each
Shortcoming, the environmental problem revealed such as the solvent recovery problem in sand solid residual after solvent extraction and solvent, hot tearing
The problem that in solution preocess, energy consumption is too high, the stability of fermentable and scale-up problems, these all make above-mentioned
Technology runs into various resistance in the middle of course of industrialization, causes it to ultimately fail to industrially and realizes scale use.
For from mineral composition, it is divided into silicate to be main mineral intergrowth material with the mineral of heavy oil field symbiosis,
Or the mineral based on carbonate.Above-mentioned all kinds of research is with for the heavy oil field rich in silicate, typically
Such as Canada's oil-sand.And the mink cell focus for carbonate type (rich in calcium carbonate etc.) is exploited the most fewer, main
If owing to the mink cell focus of this type is general and mineral has stronger active force, and making WATER-WASHING METHOD effect not
Good.Use acid wash to process this type of heavy oil field, can effectively mineral component therein be dissolved, and not
Affect the quality of mink cell focus, can preferably play the effect efficiently carrying oil.But, the weight that this technology faces
The problem is wanted to be: production process to have substantial amounts of waste liquid produce, containing materials such as abundant calcium salt, iron salt in waste liquid.
Therefore, solving wastewater problem in recovery process is also a main technical barrier.
As can be seen here, operating cost and environmental problem are the exploitations of current heavy oil field, the most glossy acid carbonate
Class oil-sand, key technical problem.To this end, patent of the present invention will propose at a kind of mainly for the problems referred to above
Manage the separation method of the heavy oil field rich in carbonate mine material.
Summary of the invention
It is an object of the invention to provide a kind of low cost, efficient, energy-conservation, may be used for processing rich in carbonate
The heavy oil field of mineral, as oil-sand, shale oil, landing oil, greasy filth etc. rich in carbonate heavy oil field
Separation and recovery method and system.
It is an object of the invention to complete by the following technical solutions:
A kind of separation and recovery method rich in carbonate heavy oil field, step is as follows
(1) mink cell focus mineral first pass through below reducing mechanism pulverizing, then mix with unitary organic acid or inorganic acid solution
Reaction, obtains containing mink cell focus foam, gas, solution, grains of sand residue mixture;
(2) mink cell focus foam is after degassing procedure, uses solvent dilution, and enters solid by the mixture after dilution
Liquid separating apparatus carries out solid-liquid separation, it is thus achieved that solvent mink cell focus mixture clear liquid, oil hydrosol and solid precipitation;
(3) gained solvent mink cell focus mixture clear liquid entrance solvent recovery unit is by solvent recovery, obtains heavy simultaneously
Oil product;Oil hydrosol and solid precipitation then enter acid dip pickle and carry out Reaction Separation, obtain solid-liquid and mix after separation
Compound, recycling design mink cell focus mixture;
(4) obtaining solidliquid mixture after (3) step solution (1) separate with step and pass through filtration, solution is through again
Add alkali remove impurity, it is thus achieved that calcium salt soln, calcium salt soln recrystallization, it is thus achieved that calcium salt;
(5) (1) above-mentioned steps obtains the precipitation merging employing alkali of grains of sand residue mixture, pickling, filter process generation
Liquid reuses after being neutralized process.
And, described is oil-sand, shale oil, landing oil or greasy filth rich in carbonate heavy oil field, in mineral
Carbonate containing is more than 10%.
And, described step (1) middle monoacid acetic acid, nitric acid, hydrochloric acid, hydroiodic acid, hydrobromic acid or formic acid etc.,
And acid solution pH value is less than 1.
And, described step (1) in mixed reactor be single-stage intermittent operation, or plural serial stage continuous way
Operation mixing reactor.
And, described step (2) middle equipment for separating liquid from solid includes the liquid-solid gravity settling device and 2~3 of 2~3 grades
The centrifugal separator of level.
And, described step (2) in the solvent that added be the petrochemical industry by-products such as toluene, gasoline, diesel oil, Petroleum
One or more of product aromatic solvent, addition is 0.5~5 times of heavy oil whip quality.
Described step (5) in filter successively, react, filter, crystallize, or be followed successively by reaction, filter, tie
Brilliant operation.
And, described step (5) middle course of reaction is to add alkali liquor to be neutralized reaction and precipitation, is added
Alkali liquor be the alkaline solutions such as sodium hydroxide solution, potassium hydroxide solution, lime water, when pH value of solution is more than 5
Time stop add alkali liquor.
And, described step (5) middle crystallization process is evaporation and crystal process, including solution concentration, crystallization, solid-liquid
Separate, be dried etc. operates.
A kind of separation and recovery method rich in carbonate heavy oil field and system, including: breaker, mixing are instead
Answer device, foam depassing unit, equipment for separating liquid from solid, solvent recovery unit, pickling reaction unit, filter dress
Put, neutralize reaction unit, crystallization apparatus, purification residual device and various material transfer equipment and pipe-line equipment,
Annexation is as follows:
Reducing mechanism material outlet connects mixing reactor, and mixed reactor is also shaped with liquid material import, liquid
Body material inlet connects acid solution storage tank, and mixed reactor is formed respectively with gas outlet, foam outlet, liquid discharge
Mouth and solid residue outlet, foam outlet connects foam depassing unit, and liquid outlet connects pickling reaction unit,
Solid residue outlet connects purification residual device, and foam depassing unit connects equipment for separating liquid from solid, is connecting pipeline
On be shaped with solvent charge door, add solvent, the oil phase outlet on equipment for separating liquid from solid top connects solvent recovery unit,
Solvent enters solvent recovery unit together with the foam after degassing, remaining drip after solvent recovery unit recycling design
Blue or green oil goes oil product refine, the liquid of equipment for separating liquid from solid bottom and solid outlet to connect pickling reaction unit after discharging,
Carrying out pickling again, the upper oil phase after pickling returns equipment for separating liquid from solid, the liquid of lower floor and solid outlet even
Taking over filter device portal, the outlet of defecator solid residue connects purification residual device, defecator liquid outlet
Connecting neutralization precipitation unit, the outlet of neutralization precipitation unit connects crystallization apparatus, and it is heavy that neutralization precipitation unit bottom is shaped with
Form sediment and export.
The unique distinction following points of the present invention:
1, the present invention uses acid solution and richness carbonato heavy oil field to carry out hybrid reaction, and raw material is convenient easily
, simple to operate, normal-temperature operation, efficiency is high, reduces cost;
2, the present invention is in mink cell focus froth treatment process, uses acid wash to process emulsion and solid precipitation,
Can well recycling design and oil, greatly reduce due to solvent or oil arrange outward the environmental problem caused;
3, mixed reactor and acid dip pickle are produced by the present invention solution and solid precipitation, use filter,
Neutralize, precipitate and the mode that crystallize processes, the various useful components in effective recovery mineral so that process without
Evilization is discharged, and reduces environmental protection treatment cost, improves economic benefit.
Accompanying drawing explanation
Fig. 1, a kind of separation and recovery method rich in carbonate heavy oil field and system flow chart;
Stock number: 1. rich in carbonate heavy oil field;2. the heavy oil field after pulverizing;3. acid solution I;
4. gas I (carbon dioxide);5. mink cell focus foam I;6. calcium salt soln II;7. solid residue (sandy soil);
8. gas II (carbon dioxide);9. mink cell focus foam II;10. fresh solvent;Mink cell focus after 11. dilutions
Foam;12. solvents-mink cell focus mixture;13. Solids-solution mixture;14. hydrocarbon class compositions;15. times
The solvent received;16. acid solutions III;17. solvents-mink cell focus foam mixture;18. gases III (carbon dioxide);
19. solidliquid mixtures;20. filtering residues (grains of sand etc. do not allow material, a small amount of);21. saline solution (calcium salt soln);
22. alkali liquor I;23. alkalinous metal precipitations;24. calcium salt solns;25. water I;26. calcium salts;27. alkali liquor
Ⅱ;28. Residual oils;29. water II;30. residual sand.
Device is numbered: A. reducing mechanism;B. mixed reactor;C. depassing unit;D. solid-liquid separation dress
Put;E. solvent recovery unit;F. pickling reaction unit;G. filter element;H. neutralization precipitation unit;I. tie
Brilliant device;J. purification residual device.
Detailed description of the invention
The invention provides a kind of apparatus and method separated for rich carbonato heavy oil field, this separation side
Method uses acid solution to react with heavy oil field, and after reaction, the mink cell focus foam of gained for solvent dilution and is consolidated
The processes such as liquid separation, pickling realize mink cell focus purification process;Gained waste reaction solution and precipitating residue then used
The methods such as filter, neutralization precipitation, crystallization are separately recovered, and finally realize mink cell focus separation and Extraction and by-product divides
The purpose that class reclaims.Mink cell focus and various mineral are not only successfully efficiently separated back by this segregation apparatus and method
Receive, accomplish almost zero-emission, and achieve economy, energy-conservation, run purpose efficiently.
Its concrete operation step is as follows:
(1) the heavy oil field size-reduced device A rich in carbonate 1 obtains little granule heavy oil field 2 after pulverizing, by
Material conveyor is delivered in mixing reactor device B, adds monoacid solution 3 and carries out hybrid reaction, dissolves
Mineral grain in heavy oil field, it is thus achieved that mink cell focus foam mixture 5, carbon dioxide 4, calcium salt soln
6 and the precipitation such as unreacted solid particles of sand 7;
(2) the mink cell focus foam 5 obtained enters, after discharging, the carbon dioxide gas that depassing unit C will contain in foam
Body 8 removes, and adds solvent 10 and be diluted the foam after degasification in mink cell focus foam 9 after degassing;
Mink cell focus foam 11 after dilution enters equipment for separating liquid from solid D, is divided into upper oil phase clear liquid 12 (solvent and weight
Matter oil mixture), oil hydrosol and solid phase precipitate 13;Upper oil phase clear liquid 12 extraction also enters solvent
Recovery unit E separates, and recycling design 15 also obtains hydrocarbon class composition 14, and hydrocarbon class composition is through rectification
The operations such as separation, it is thus achieved that product oil;
(3) after oil hydrosol and solid sediment 13 are discharged, entrance pickling reaction unit F carries out pickling processes (acid
Wash reaction unit and add in mixed reactor (B) liquid or fresh monoacid solution 16, institute more than part monoacid
Upper oil phase 17 is back to equipment for separating liquid from solid D and carries out secondary separation;Obtain gas 18 to collect or discharge,
The solidliquid mixture 19 that the solution produced after pickling and precipitation are formed, enters filter element G and filters, it is thus achieved that no
Saline solution 21 containing solid and solid filter residue 20;
The most above-mentioned solution 21 is input in neutralization precipitation unit H, adds alkali liquor 22 and removes hetero atom alkali gold
Belonging to precipitation 23, gained calcium salt soln 24 enters crystallization apparatus I and is evaporated crystallization, it is thus achieved that product crystals of calcium salts
26, the water 25 of evaporation gained reclaims;
(5) the solid filter residue 20 that the precipitate 7 in mixed reactor and filter element obtain is separately added into residue
Clean unit J mixes, residue 30 safety dumping obtained after adding the washing of suitable aqueous alkali 27, it is thus achieved that residual
Oil 28 reclaims, and remaining aqueous solution 29 discharges.
The present invention use acid solution be unitary organic acid or mineral acid, as acetic acid, nitric acid, hydrochloric acid, hydroiodic acid,
The mixture of one or more of hydrobromic acid, formic acid etc., and acid solution pH value is less than 1.
Described acid solution is 1:3-10 with the solid-to-liquid ratio of heavy oil field.
In the present invention, mixed reactor is single-stage intermittent operation, or plural serial stage continuous way operation hybrid reaction
Device.
In the present invention, equipment for separating liquid from solid includes the liquid-solid gravity separator of 2~3 grades and 2~3 grades centrifugal
Separator, separates such as centrifuge or suspension separates.
In the present invention, the solvent for asphalt foam dilution is the fragrance hydrocarbon systems such as toluene, gasoline, diesel oil, Petroleum
The mixture of one or more of row, use ratio is 0.5~5 times of foam quality.
The alkali liquor used is the alkaline solutions such as sodium hydroxide solution, potassium hydroxide solution, lime water, and concentration is
0.01-10mol/L。
The present invention is realized by following equipment and technical scheme:
A kind of separation and recovery system rich in carbonate heavy oil field, specifically includes: breaker, hybrid reaction
Device, foam depassing unit, equipment for separating liquid from solid, solvent recovery unit, pickling reaction unit, defecator,
Neutralize reaction unit, crystallization apparatus, purification residual device and various material transfer equipment and pipe-line equipment.Connect
Relation is as follows:
Reducing mechanism material outlet connects mixing reactor, and mixed reactor is also shaped with liquid material import, liquid
Body material inlet connects acid solution storage tank, and mixed reactor is formed respectively with gas outlet, foam outlet, liquid discharge
Mouth and solid residue outlet, foam outlet connects foam depassing unit, and liquid outlet connects pickling reaction unit,
Solid residue outlet connects purification residual device, and foam depassing unit connects equipment for separating liquid from solid, is connecting pipeline
On be shaped with solvent charge door, add solvent, the oil phase outlet on equipment for separating liquid from solid top connects solvent recovery unit,
Solvent enters solvent recovery unit together with the foam after degassing, remaining drip after solvent recovery unit recycling design
Blue or green oil goes oil product refine, the liquid of equipment for separating liquid from solid bottom and solid outlet to connect pickling reaction unit after discharging,
Carrying out pickling again, the upper oil phase after pickling returns equipment for separating liquid from solid, the liquid of lower floor and solid outlet even
Taking over filter device portal, the outlet of defecator solid residue connects purification residual device, defecator liquid outlet
Connecting neutralization precipitation unit, the outlet of neutralization precipitation unit connects crystallization apparatus, and it is heavy that neutralization precipitation unit bottom is shaped with
Form sediment and export.
The concrete operation step of process implementing:
Within rich carbonato heavy oil field size-reduced device A is crushed to 5cm, material conveyor deliver to
Mixing reactor device B carries out hybrid reaction with the pH acid solution more than 1.Mink cell focus mineral are dissolved
Grain, it is thus achieved that mink cell focus foam mixture, gas, solution and precipitation.The mink cell focus foam obtained is discharged into removing
The carbon dioxide that contains in foam is removed by device of air, is subsequently adding and is equivalent to foam volume 0.5~5 times
Foam after degasification is diluted by solvent;Foam after dilution enter equipment for separating liquid from solid be divided into oil phase clear liquid,
Oil hydrosol and solid bulk precipitation;Oil phase clear liquid extraction also enters solvent recovery unit and separates, recycling design
And obtain hydrocarbon class composition;Oil hydrosol and solid sediment enter descaling bath after discharging and carry out pickling processes, institute
Upper oil phase is back to equipment for separating liquid from solid and separates;After pickling produce solution and precipitation with from mixing
The solution of reaction unit mixes and filters, it is thus achieved that without the solution of solid;Above-mentioned solution adds alkali liquor and removes miscellaneous
Atom, gained calcium salt soln is evaporated crystallization, it is thus achieved that product;Precipitate in mixed reactor and pickling
With safety dumping after suitable soda lye wash after precipitate mixing in solution in groove.
Below, present invention following example are illustrated, but is not limited to following example.
Embodiment 1:
A kind of separation and recovery method rich in carbonate heavy oil field and system, step is as follows:
(1) the oil-sand 15kg (carbonate content 42%, maximum particle diameter 0.5cm) pulverized through reducing mechanism A send
Entering in mixing-reactor B with the hydrochloric acid that pH is 1 according to solid-to-liquid ratio is that 1:30 (mass ratio) fills under room temperature
Divide mixing and react 1 hour.
The most above-mentioned reaction gained asphalt foam adds the Petroleum of 0.5 times of foam quality after C degasification operates and enters
Row solid-liquid separation (two grades of sedimentations and two-stage centrifugal D), in separating obtained upper oil phase clear liquid, moisture is less than
3.5%, solid content is less than 1.5%, enters in E and separates, recycling design, obtains coal tar product simultaneously
14, bitumen recovery rate 99.1%.
(3) the emulsion of equipment for separating liquid from solid D gained and solid precipitation are sent to descaling bath F washing, gained waste liquid and
Residue precipitation, after G filters, adds sodium hydroxide solution and is neutralized precipitation at H, filtered by tan precipitate
Going out, gained solution enters in I and crystallizes.
(4) the solid residue obtained from mixed reactor B and defecator G enters in purification residual device J
Using neutralization to carry out purified treatment, sandy soil and oil residues are reclaimed in classification.
Final acquisition calcium chloride crystals purity 99.1%, hydrated ferric oxide. content 92.5% in tan precipitate, residue is solid
Body is neutral.
Embodiment 2:
A kind of separation and recovery method rich in carbonate heavy oil field and system, step is as follows:
(1) the oil-sand 15kg (carbonate content 61%, maximum particle diameter 5cm) pulverized through reducing mechanism A sends into
Mixing-reactor B is that 1:3 (mass ratio) is in often with the hydrobromic acid that concentration is 2 mol/L according to solid-to-liquid ratio
It is sufficiently mixed under temperature, reacts 120min.
(2) gained asphalt foam gasoline of 5 times of volumes of addition after C degasification operates carries out solid-liquid separation (three
Level sedimentation and three grades of centrifugal D), in separating obtained upper oil phase clear liquid, moisture is less than 1.5%, and solid content is little
In 1.5%, enter in E and separate, recycling design, obtain coal tar product 14, bitumen recovery rate simultaneously
98.7%.
(3) the emulsion of equipment for separating liquid from solid D gained and solid precipitation are sent to descaling bath F washing, gained waste liquid and
Residue precipitation is after G filters, and filtrate enters in neutralization precipitation device H, and it is heavy that addition lime water is neutralized
Forming sediment, leached by tan precipitate, gained solution carries out being evaporated crystallization in entrance I.
(4) the solid residue obtained from mixed reactor B and defecator G enters in purification residual device J
Using neutralization to carry out purified treatment, sandy soil and oil residues are reclaimed in classification.
Final acquisition calcium chloride crystals purity 99.8%, hydrated ferric oxide. content 94.3% in tan precipitate, residue is solid
Body is neutral.
Embodiment 3:
A kind of separation and recovery method rich in carbonate heavy oil field and system, step is as follows:
(1) the greasy filth 15kg (carbonate content 56%, maximum particle diameter 1.5cm) pulverized through reducing mechanism A send
Enter in mixing-reactor B with the nitric acid that concentration is 3 mol/L according to solid-liquid ratio be 1:3 (mass ratio) in
It is sufficiently mixed under room temperature, reacts 120min.
Gained asphalt foam add after C degasification operates 5 times of volumes Petroleum and kerosene (volume ratio,
1:1) carrying out solid-liquid separation (two-stage sedimentation and three grades of suspension D), in separating obtained upper oil phase clear liquid, moisture contains
Amount is less than 1.5%, and solid content is less than 1.5%, enters in E and separates, and recycling design obtains Colophonium simultaneously
Oil product 14, bitumen recovery rate 99.3%.
(3) the emulsion of equipment for separating liquid from solid D gained and solid precipitation are sent to descaling bath F washing, gained waste liquid and
Residue precipitation is after G filters, and filtrate enters in neutralization precipitation device H, and it is heavy that addition lime water is neutralized
Forming sediment, leached by tan precipitate, gained solution carries out being evaporated crystallization in entrance I.
(4) the solid residue obtained from mixed reactor B and defecator G enters in purification residual device J
Using neutralization to carry out purified treatment, sandy soil and oil residues are reclaimed in classification.
Final acquisition calcium nitrate crystal purity 97.8%, hydrated ferric oxide. content 93.7% in tan precipitate, residue is solid
Body is neutral.
Embodiment 4:
A kind of separation and recovery method rich in carbonate heavy oil field and system, step is as follows:
(1) the oil shale 15kg (carbonate content 52%, maximum particle diameter 5cm) pulverized through reducing mechanism A send
Enter in mixing-reactor B with the acetic acid that concentration is 5 mol/L according to solid-liquid ratio be 1:3 (mass ratio) in
At 65 DEG C mix, reaction 30min, mixed reactor B be two-stage series connection, i.e. one-level be hybrid reaction,
Another level is flotation.
(2) gained asphalt foam toluene of 5 times of volumes of addition after C degasification operates carries out solid-liquid separation (two
Level sedimentation separates D with two-stage suspension), in separating obtained upper oil phase clear liquid, moisture is less than 1.2%, admittedly contain
Amount, less than 1.5%, enters in E and separates, recycling design, obtains coal tar product 14 simultaneously, and Colophonium returns
Yield 99.7%.
(3) the emulsion of equipment for separating liquid from solid D gained and solid precipitation are sent to descaling bath F washing, gained waste liquid and
Residue precipitation is after G filters, and filtrate enters in neutralization precipitation device H, and it is heavy that addition lime water is neutralized
Forming sediment, leached by tan precipitate, gained solution carries out being evaporated crystallization in entrance I.
(4) the solid residue obtained from mixed reactor B and defecator G enters in purification residual device J
Using neutralization to carry out purified treatment, sandy soil and oil residues are reclaimed in classification.
Final acquisition calcium acetate purity 97.5%, hydrated ferric oxide. content 93.4% in tan precipitate, in residue solid
Property.
Embodiment 5:
A kind of separation and recovery method rich in carbonate heavy oil field and system, step is as follows:
(1) the oil-sand 15kg (carbonate content 52%, maximum particle diameter 3cm) pulverized through reducing mechanism A sends into
Mixing-reactor B is that 1:6 (mass ratio) is in 25 DEG C with the formic acid that concentration is 1 mol/L according to solid-liquid ratio
Under be sufficiently mixed, reaction 30min, mixed reactor B be two-stage series connection, i.e. two-stage mixing reactor hand over
For carrying out reaction and stratification operation.
(2) gained asphalt foam kerosene of 5 times of volumes of addition after C degasification operates carries out solid-liquid separation (two
Level sedimentation separates D with two-stage suspension), in separating obtained upper oil phase clear liquid, moisture is less than 2.5%, admittedly contain
Amount, less than 1.5%, enters in E and separates, recycling design, obtains coal tar product 14 simultaneously, and Colophonium returns
Yield 99.6%.
(3) the emulsion of equipment for separating liquid from solid D gained and solid precipitation are sent to descaling bath F washing, gained waste liquid and
Residue precipitation is after G filters, and filtrate enters in neutralization precipitation device H, and it is heavy that addition lime water is neutralized
Forming sediment, leached by tan precipitate, gained solution carries out being evaporated crystallization in entrance I.
(4) the solid residue obtained from mixed reactor B and defecator G enters in purification residual device J
Using neutralization to carry out purified treatment, sandy soil and oil residues are reclaimed in classification.
Final acquisition calcium formate purity 98.9%, coal tar solid content is less than 1%, and residue solid is neutral.
A kind of apparatus and method separated rich in carbonate heavy oil field that the present invention proposes, by preferably implementing
Example is described, and person skilled substantially can be to this in without departing from present invention, spirit and scope
Structure described in literary composition and technical method is modified or suitably changes and combines, realizes the technology of the present invention.Especially
It is pointed out that all similar replacements and change apparent to those skilled in the art,
They are considered as being included in present invention spirit, scope and content.
Claims (10)
1. the separation and recovery method rich in carbonate heavy oil field, it is characterised in that: step is as follows
(1) mink cell focus mineral first pass through below reducing mechanism pulverizing, then mix with unitary organic acid or inorganic acid solution
Reaction, obtains containing mink cell focus foam, gas, solution, grains of sand residue mixture;
(2) mink cell focus foam is after degassing procedure, uses solvent dilution, and enters solid by the mixture after dilution
Liquid separating apparatus carries out solid-liquid separation, it is thus achieved that solvent mink cell focus mixture clear liquid, oil hydrosol and solid precipitation;
(3) gained solvent mink cell focus mixture clear liquid entrance solvent recovery unit is by solvent recovery, obtains heavy simultaneously
Oil product;Oil hydrosol and solid precipitation then enter acid dip pickle and carry out Reaction Separation, obtain solid-liquid and mix after separation
Compound, recycling design mink cell focus mixture;
(4) obtaining solidliquid mixture after (3) step solution (1) separate with step and pass through filtration, solution is through again
Add alkali remove impurity, it is thus achieved that calcium salt soln, calcium salt soln recrystallization, it is thus achieved that calcium salt;
(5) (1) above-mentioned steps obtains the precipitation merging employing alkali of grains of sand residue mixture, pickling, filter process generation
Liquid reuses after being neutralized process.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: institute is oil-sand, shale oil, landing oil or greasy filth rich in carbonate heavy oil field, and in mineral, carbonate contains
Amount is more than 10%.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (1) middle monoacid acetic acid, nitric acid, hydrochloric acid, hydroiodic acid, hydrobromic acid or formic acid etc., and acid is molten
Liquid pH value is less than 1.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (1) in mixed reactor be single-stage intermittent operation, or the operation of plural serial stage continuous way is mixed
Close reactor.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (2) middle equipment for separating liquid from solid includes the liquid-solid gravity settling device of 2~3 grades and 2~3 grades centrifugal
Formula segregation apparatus.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (2) in the solvent that added be the Some Petrochemical Byproducts aromatic hydrocarbons such as toluene, gasoline, diesel oil, Petroleum
One or more of solvent, addition is 0.5~5 times of heavy oil whip quality.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (3) in the part that pickle is step (1) pickle or fresh pickle, institute after pickling
Obtain upper oil phase and be recycled to equipment for separating liquid from solid;Described step (4) in filter successively, react, filter, crystallize,
Or it is followed successively by reaction, the operation filtered, crystallize.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (4) middle course of reaction is to add alkali liquor to be neutralized reaction and precipitation, the alkali liquor added
For alkaline solutions such as sodium hydroxide solution, potassium hydroxide solution, lime water, stop when pH value of solution is more than 5
Add alkali liquor.
Separation and recovery method rich in carbonate heavy oil field the most according to claim 1, its feature exists
In: described step (4) in crystallization process be evaporation and crystal process, including solution concentration, crystallization, solid-liquid separation,
It is dried and waits operation.
10. the separation and recovery system rich in carbonate heavy oil field, it is characterised in that including: broken dress
Put, mixed reactor, foam depassing unit, equipment for separating liquid from solid, solvent recovery unit, pickling reaction dress
Put, defecator, neutralization reaction unit, crystallization apparatus, purification residual device and various material transfer equipment and
Pipe-line equipment, annexation is as follows:
Reducing mechanism material outlet connects mixing reactor, and mixed reactor is also shaped with liquid material import, liquid
Body material inlet connects acid solution storage tank, and mixed reactor is formed respectively with gas outlet, foam outlet, liquid discharge
Mouth and solid residue outlet, foam outlet connects foam depassing unit, and liquid outlet connects pickling reaction unit,
Solid residue outlet connects purification residual device, and foam depassing unit connects equipment for separating liquid from solid, is connecting pipeline
On be shaped with solvent charge door, add solvent, the oil phase outlet on equipment for separating liquid from solid top connects solvent recovery unit,
Solvent enters solvent recovery unit together with the foam after degassing, remaining drip after solvent recovery unit recycling design
Blue or green oil goes oil product refine, the liquid of equipment for separating liquid from solid bottom and solid outlet to connect pickling reaction unit after discharging,
Carrying out pickling again, the upper oil phase after pickling returns equipment for separating liquid from solid, the liquid of lower floor and solid outlet even
Taking over filter device portal, the outlet of defecator solid residue connects purification residual device, defecator liquid outlet
Connecting neutralization precipitation unit, the outlet of neutralization precipitation unit connects crystallization apparatus, and it is heavy that neutralization precipitation unit bottom is shaped with
Form sediment and export.
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