CN106433605B - A kind of oil shale in-situ increases hole activating treatment agent and preparation method thereof - Google Patents
A kind of oil shale in-situ increases hole activating treatment agent and preparation method thereof Download PDFInfo
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- CN106433605B CN106433605B CN201510472598.9A CN201510472598A CN106433605B CN 106433605 B CN106433605 B CN 106433605B CN 201510472598 A CN201510472598 A CN 201510472598A CN 106433605 B CN106433605 B CN 106433605B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
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Abstract
The invention belongs to oil shale in-situs to exploit field, provide a kind of oil shale in-situ increasing hole activating treatment agent and the preparation method of the inorganic agent.The raw material of the inorganic agent includes: sour 5%-28%, cobalt salt and/or nickel salt 0.1%-1%, corrosion inhibiter 1%-3%, mutual solvent 0.1%-20%, water 6.2%-52% based on mass percentage.The present invention also provides the preparation methods of the inorganic agent, including the acid, cobalt salt and/or nickel salt, corrosion inhibiter and mutual solvent are added to the water and stirred to get.Oil shale in-situ is increased hole, improves permeability and the synergy integration of in-situ heat conversion catalyst by the inorganic agent, can be increased oil shale porosity, be increased oil shale oil-collecting ratio under the conditions of identical temperature and time.And preparation method is simple, can prepare in make-up station, can also directly prepare at the scene, it is easy to use.
Description
Technical field
The invention belongs to oil shale in-situs to exploit field, and in particular to a kind of oil shale in-situ increasing hole activating treatment agent, with
And the preparation method of the inorganic agent.
Background technique
Oil shale takes over one of energy as the important of conventional gas and oil, its development and utilization are increasingly by countries in the world
Pay attention to.According to statistics, world's oil shale oil stock number is about 411,000,000,000 tons at present, and China's shale oil resource is about 476.44 hundred million
Ton, the ranking whole world second is only second to the U.S..China's oil shale resources are buried relatively deeply, and oil shale average thickness is about 20-30m, and
Accompany sandstone, mud stone etc., and quite a few is lean ore (account for about 45.4%) of the oil content less than 5% more, and oil content is big
Rich ore in 10% is less (17.6%), and the resource between 5%-10% oil content accounts for 37%.
The mining method of oil shale can be divided into ground destructive distillation and two kinds of in-situ retorting, although ground destructive distillation have technique at
Ripe, the advantages that heating cycle is short, investment is quick, but environmental pollution is extremely serious, considerable damage soil, residue treatment wave again
Take a large amount of water resource, while very big pollution is also resulted in water quality and air, also needs to carry out backfilling working after exploitation.With
The increase of environmental protection pressure, oil shale in-situ exploitation have become the inexorable trend of the following oil shale commercialization large-scale development.
A large amount of research has been carried out in terms of oil shale in-situ exploitation by each major oil companies, foreign countries of representative of shell.Shell
Board has successfully produced shale in the green river area in the U.S. using electric heating ICP (In-situ Conversion Process) technology
Oil, but electric-heating technology heating speed is slow, and heating cycle is long, generally requires 2-4, need to consume a large amount of electric energy.Because no
The supplement of outside energy, tar productivity is lower to lead to deficiency in economic performance.
Fluid heating technique because heating speed is fast, heating cycle is short, the advantages that carbonization gas can be made full use of due to closed extensively
Note.But oil shale porosity is low, and permeability is extremely low, and hot fluid can not inject rock stratum, it is necessary to carry out reservoir reconstruction early period, make its tool
There is certain permeability.Common concern at present is hydraulic fracturing and explosion fracturing technology, but the crack that hydraulic fracturing is formed can
The direct channelling of fluid can be led to inject to producing well, so that the thermal efficiency is low, most of rock stratum can not be heated to kerogen cracking
Temperature (350 DEG C or more).Although explosion fracturing can form multiple cracking around nearly well, process range is small, and crack is to hot-fluid
The surface area contacted with oil shale that body provides is relatively small, and oil shale heating surface area is small, and heating speed is relatively low, oil shale
Converted in-situ speed is slow, low efficiency.
It, can in order to increase oil shale heating surface area in oil shale in-situ heating recovery process, improve oil shale heating efficiency
To carry out the processing such as increasing hole, activation to oil shale formation.However the processing base that oil shale is carried out in domestic prior art at present
It is all confined to that oil shale particle is carried out in oil shale retort process the processing such as to be catalyzed in sheet, to improve oil shale oil
The quality and yield of product do not refer to that any substance of injection in situ carries out increasing hole, activation or catalysis etc. to oil shale formation.State
In outer a small amount of patent (such as patent AU2011348120, US8727000) mention can will be containing the anti-of oxidant, organic solvent etc.
It answers liquid to be injected into oil shale formation, contacts it with subterranean oil shale, and react, separate kerogen from oil shale
Out, but at present have no that injection increases the relevant report of the inorganic agent of hole and activation for oil shale in-situ.
Summary of the invention
The present invention provides a kind of oil shale in-situ increasing hole, activating treatment agent.By rationally compounding each component, to oil shale
Increasing hole in situ is carried out, its permeability is improved, changes simultaneously the reaction path of kerogen pyrolytic process, accelerate conversion rate, reach
The purpose for reducing thermal energy consumption, improving production efficiency and oil productivity.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of oil shale in-situ increasing hole activating treatment agent, raw material includes: sour 5%-28%, cobalt based on mass percentage
Salt and/or nickel salt 0.1%-1%, corrosion inhibiter 1%-3%, mutual solvent 0.1%-20%, water 6.2%-52%.
In a specific embodiment of the present invention, raw material is calculated as by mass percentage: sour 5%-28%, cobalt salt and/or
Nickel salt 0.1%-1%, corrosion inhibiter 1%-3%, mutual solvent 0.1%-20%, remaining is water.
In a specific embodiment of the present invention, the acid is selected from hydrochloric acid, hydrofluoric acid, phosphoric acid, sulfuric acid, nitric acid, fluoboric acid, fluorine
At least one of silicic acid, formic acid and acetic acid act on to carry out corrosion and reaming to oil shale layer.Two or more acid combinations make
More preferable with effect, preferred combination includes hydrochloric acid and the combination of hydrofluoric acid, the combination of hydrochloric acid and fluoboric acid, hydrochloric acid and fluosilicic acid
Combination, hydrochloric acid and hydrofluoric acid and the combination of acetic acid etc.." acid is calculated as 5%-28% by mass percentage " is meant that pure solute
Mass percentage in inorganic agent, if content of hydrochloric acid is that 5%-28% refers to that quality percentage of the hydrogen chloride in inorganic agent contains
Amount is 5%-28%.Above each acid is the chemically pure reagent that can industrially buy, and has known concentration.
In a specific embodiment of the present invention, the cobalt salt is selected from cobaltous sulfate, cobalt chloride, cobalt carbonate, cobaltous formate and acetic acid
At least one of cobalt, the nickel salt are selected from least one of nickel chloride, nickel sulfide, nickel sulfate and nickel sulfamic acid.It is described
The effect of cobalt salt and/or nickel salt is that catalyst is used as in increasing hole and activation process, promotes the organic matter decomposition in oil shale layer.
In a specific embodiment of the present invention, the corrosion inhibiter is selected from formaldehyde, o-xylene thiourea, sodium alkyl sulfonate and chlorine
Change at least one of benzyl pyridine, act on increasing hole and activation process to make oil shale and steadily occur, mitigates acid to metal tube
The corrosion of material.
In a specific embodiment of the present invention, the general formula of the mutual solvent are as follows: R-O- (- CH2CH2O-)n-H.In formula, R is
C1-C8Alkyl, preferably C1-C8Alkyl, more preferably C1-C4Alkyl；N is the integer of 0-4.The mutual solvent preferably selects
From methanol (R C1, n 0), ethyl alcohol (R C2, n 0), propyl alcohol (R C3, n 0), butyl glycol ether (R C4, n 1), two
Ethylene glycol ethyl ether (R C2, n 2), butyl (R C4, n 2) and triethylene glycol butyl ether (R C4, n 3) in
At least one, act on for make water phase base fluid in oil shale layer oil-wetted surface and organic matter therein come into full contact with.
The present invention also provides the preparation methods of above-mentioned inorganic agent, including by the acid, cobalt salt and/or nickel salt, corrosion inhibiter
It is added to the water with mutual solvent and stirs to get.
In a specific embodiment of the present invention, the method includes be added into part or all of desired amount of water acid,
Cobalt salt and/or nickel salt, corrosion inhibiter and mutual solvent, it is stirring while adding, if necessary, then plus remaining water to design quantity, stirring
The inorganic agent is obtained after uniformly.It is preferred that first above-mentioned raw materials are dissolved in the water for accounting for total Water 2/3~4/5, after being sufficiently stirred again
Remaining water is added, keeps dissolution more abundant.
Oil shale in-situ provided by the invention increases hole activating treatment agent, and oil shale in-situ is increased hole, improves permeability and original
Position thermal transition catalysis synergy integration, can increase oil shale porosity, receive oil shale under the conditions of identical temperature and time
Oil cut rate increases.And the inorganic agent preparation method is simple, can prepare, can also be directly prepared at the scene in make-up station, it is easy to use.
Specific embodiment
Below by embodiment, present invention be described in more detail.
Embodiment 1
A kind of oil shale in-situ increasing hole activating treatment agent, raw material is by mass percentage are as follows: hydrochloric acid 12%, hydrofluoric acid
1.5%, cobalt chloride 0.1%, formaldehyde 1%, butyl glycol ether 12.4%, water 73%.Preparation method are as follows: according to formula concentration meter
Raw material dosage needed for calculating first measures 30.00 parts by weight of clear water, and the technical hydrochloric acid that mass concentration is 36% is slowly added into clear water
3.75 parts by weight of industrial hydrofluoric acid, 12.40 parts by weight of butyl glycol ether, quality that 33.33 parts by weight, mass concentration are 40% are dense
Industrial formol 2.70 parts by weight, CoCL2 6H2O 0.18 parts by weight of the degree for 37%, it is stirring while adding, after the solid is completely dissolved
17.64 parts by weight of clear water are added, obtain the inorganic agent after mixing evenly.
Embodiment 2
A kind of oil shale in-situ increasing hole activating treatment agent, raw material is by mass percentage are as follows: hydrofluoric acid 5%, acetic acid
15%, cobalt acetate 1%, formaldehyde 2%, butyl glycol ether 6%, water 71%.Preparation method are as follows: needed for being calculated according to formula concentration
Raw material dosage first measures 40 parts by weight of clear water, and 12.50 weight of industrial hydrofluoric acid that mass concentration is 40% is slowly added into clear water
Measure part, 15.31 parts by weight of glacial acetic acid that mass concentration is 98%, 6.00 parts by weight of ethylene glycol monobutyl ether, mass concentration 37%
5.41 parts by weight of industrial formol, four acetate hydrate cobalts, 1.41 parts by weight, it is stirring while adding, add after the solid is completely dissolved
19.37 parts by weight of clear water, obtain the inorganic agent after mixing evenly.
Embodiment 3
A kind of oil shale in-situ increasing hole, activating treatment agent, raw material is by mass percentage are as follows: hydrochloric acid 12%, hydrofluoric acid
3%, acetic acid 10%, nickel sulfamic acid 0.5%, formaldehyde 3%, ethyl alcohol 18%, water 53.5%.Preparation method are as follows: according to formula
Raw material dosage needed for concentration calculation measures 22.22 parts by weight of clear water, and the industry that mass concentration is 36% is slowly added into clear water
The glacial acetic acid that 7.5 parts by weight of industrial hydrofluoric acid that 33.33 parts by weight of hydrochloric acid, mass concentration are 40%, mass concentration are 98%
10.20 parts by weight, 18.00 parts by weight of ethyl alcohol, 8.11 parts by weight of industrial formol that mass concentration is 37%, four hydration sulfamic acids
0.64 parts by weight of nickel, it is stirring while adding, it is all dissolved to solid, obtains the inorganic agent after mixing evenly.
Inorganic agent performance test process is as follows: taking particle size range is the oil shale particle sample 30g of 3.35-4.75mm, is added
The inorganic agent 100g for entering embodiment 1-3 preparation, reacts 2 hours under 40 DEG C of environment；Inorganic agent is poured out after having reacted, and is washed with clear water
Sample is placed in 105 DEG C of baking ovens 4 hours dry by absolute oil shale samples；Test oil shale samples are under normal temperature and pressure conditions
Porosity, and the oil-collecting ratio after being heated 15 hours under the conditions of 350 DEG C.The results are shown in Table 1.
Comparative example 1
Taking particle size range is the oil shale particle sample 30g of 3.35-4.75mm, and sample is placed in 105 DEG C of baking ovens dry 4
Hour, the porosity of test oil shale samples under normal temperature and pressure conditions, and the receipts after being heated 15 hours under the conditions of 350 DEG C
Oil cut rate.The results are shown in Table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| Porosity (%) | 28 | 29 | 29 | 15 |
| Oil-collecting ratio (%) | 37 | 39 | 40 | 29 |
As shown in Table 1, under the same conditions, embodiment 1-3 is compared acid extraction with comparative example, oil shale hole
Degree increases, and oil-collecting ratio significantly improves.Show that inorganic agent of the invention can carry out oil shale to increase hole transformation, improve permeability, together
When accelerate oil shale thermal transition speed, realize catalysis synergistic effect.
It should be noted that embodiment described above for explaining only the invention, is not constituted to of the invention any
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word used in it is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to particular case disclosed in it, on the contrary, this hair
It is bright to can be extended to other all methods and applications with the same function.
Claims (11)
1. a kind of oil shale in-situ increases hole activating treatment agent, raw material includes: sour 5%-28%, cobalt salt based on mass percentage
And/or nickel salt 0.1%-1%, corrosion inhibiter 1%-3%, mutual solvent 0.1%-20%, water 6.2%-52%；
Wherein, it is described acid in hydrochloric acid, hydrofluoric acid, phosphoric acid, sulfuric acid, nitric acid, fluoboric acid, fluosilicic acid, formic acid and acetic acid extremely
It is two kinds few.
2. inorganic agent according to claim 1, which is characterized in that the cobalt salt be selected from cobaltous sulfate, cobalt chloride, cobalt carbonate,
At least one of cobaltous formate and cobalt acetate.
3. inorganic agent according to claim 1 or 2, which is characterized in that the nickel salt is selected from nickel chloride, nickel sulfide, sulfuric acid
At least one of nickel and nickel sulfamic acid.
4. inorganic agent according to claim 1 or 2, which is characterized in that the corrosion inhibiter is selected from formaldehyde, ortho-xylene sulphur
At least one of urea, sodium alkyl sulfonate and zephiran chloride pyridine.
5. inorganic agent according to claim 1 or 2, which is characterized in that the general formula of the mutual solvent be R-O- (-
CH2CH2O-)n- H, wherein R is C1-C8Alkyl；N is the integer of 0-4.
6. inorganic agent according to claim 5, which is characterized in that wherein R is C1-C8Alkyl.
7. inorganic agent according to claim 6, which is characterized in that wherein R is C1-C4Alkyl.
8. inorganic agent according to claim 5, which is characterized in that the mutual solvent is selected from methanol, ethyl alcohol, propyl alcohol, second two
At least one of alcohol butyl ether, diethylene glycol ether, butyl and triethylene glycol butyl ether.
9. a kind of prepare according to claim 1 to the method for inorganic agent described in any one of 8, including by the acid, cobalt salt and/or
Nickel salt, corrosion inhibiter and mutual solvent, which are added to the water, to be stirred to get.
10. according to the method described in claim 9, it is characterized in that, by the acid, cobalt salt and/or nickel salt, corrosion inhibiter and dissolving each other
Agent is first dissolved in the water for accounting for total Water 2/3~4/5, and remaining water is added after stirring.
11. inorganic agent described in any item of the claim 1 to 8 increases the application in the activation of hole in oil shale in-situ.
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2015
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| US20120160486A1 (en) * | 2010-12-22 | 2012-06-28 | Chevron U.S.A. Inc. | In-situ kerogen conversion and recovery |
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