CN107325795A - Water-fastness swollen clay stabilizer of contracting and preparation method thereof - Google Patents
Water-fastness swollen clay stabilizer of contracting and preparation method thereof Download PDFInfo
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- CN107325795A CN107325795A CN201710635559.5A CN201710635559A CN107325795A CN 107325795 A CN107325795 A CN 107325795A CN 201710635559 A CN201710635559 A CN 201710635559A CN 107325795 A CN107325795 A CN 107325795A
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- mother liquor
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- fastness
- contracting
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- C—CHEMISTRY; METALLURGY
- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- C—CHEMISTRY; METALLURGY
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
Abstract
It is a kind of water-fastness swollen clay stabilizer of contracting and preparation method thereof, it is obtained as follows the present invention relates to swollen dose of technical field of contracting:12/14 tertiary amines are first synthesized quaternary ammonium salt mother liquor with hydrochloric acid by the first step, then are added oxidant I into quaternary ammonium salt mother liquor and obtained mother liquor I;Second step, hexamethylenetetramine hydrochloric acid mother liquor is synthesized with hydrochloric acid by hexamethylenetetramine, then is added aluminium ion crosslinking agent into hexamethylenetetramine hydrochloric acid mother liquor and obtained mother liquor II;3rd step, chooses and adjusts pH value to be to obtain the water-fastness swollen clay stabilizer of contracting after mother liquor I, mother liquor II, polyquaternium, oxidant II, polymer, zirconium oxychloride, zinc acetate, solvent, surfactant mixing with monoethanolamine.The present invention by compounding the need for synthesize certain density mother liquor, then compound the swollen clay stabilizer of water-fastness contracting for obtaining the present invention, not only with the swollen performance that preferably contracts, while having preferable wash durability, preparation process is simply easily implemented, functional.
Description
Technical field
It is a kind of water-fastness swollen clay stabilizer of contracting and preparation method thereof the present invention relates to swollen dose of technical field of contracting.
Background technology
The clay stabilizer species used on current oil field is various, and static preventive effect of expansion can reach technical indicator, 0.5%
The aqueous solution(Solid >=80.0%, liquid >=70.0%)Effect is uneven.The anti-swollen technology that research is water-fastness, contracting is swollen lacks, and lacks
Few not only preventive effect of expansion well have again contract swollen effect and can be water-fastness clay stabilizer, a kind of medicament of exclusive use is difficult to reach multiple
Effect, several single preferable composite reagent Comparisions of effect are difficult, and effect is also undesirable.
The content of the invention
The invention provides swollen clay stabilizer of the water-fastness contracting of one kind and preparation method thereof, overcome above-mentioned prior art it
Deficiency, it can effectively solve to lack at present not only preventive effect of expansion well and have asking for contract swollen effect and the water-fastness clay stabilizer of energy
Topic.
One of technical scheme is realized by following measures:A kind of water-fastness swollen clay stabilizer of contracting,
Obtain as follows:The first step, first by 12/14 tertiary amines and concentration for 31% to 38% hydrochloric acid solution with mol ratio 1:
1.5 are mixed into quaternary ammonium salt mother liquor, then add the oxidant I of quaternary ammonium salt mother liquor 0.07% to 0.12% into quaternary ammonium salt mother liquor, in temperature
Spend and obtain mother liquor I to react 30min to 35min under the conditions of 15 DEG C to 20 DEG C;
Second step, by hexamethylenetetramine and concentration for 36% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into six first
Urotropine hydrochloric acid mother liquor, then aluminium ion crosslinking agent is added into hexamethylenetetramine hydrochloric acid mother liquor, wherein in aluminium ion crosslinking agent
Aluminium ion accounts for the 0.1% to 1% of hexamethylenetetramine hydrochloric acid mother liquor, then selects the mode of gradient increased temperature to be reacted:First heat up
To 20 DEG C to 30 DEG C progress first set reactions, the first set reaction time be 30min to 35min, then be warming up to 45 DEG C to 55 DEG C and enter
The secondary response of row second, second reaction time be 30min to 35min, finally obtain mother liquor II;
3rd step, by weight meter choose I 19 parts to 39 parts of raw material mother liquor, II 9 parts to 29 parts of mother liquor, molecular weight be 300,000 to
500000 0.5 part to 5 parts of polyquaternium, II 0.1 parts to 1 part of oxidant, 0.01 part to 0.1 part of polymer, 1.7 parts of zirconium oxychloride
To 9.7 parts, 0.6 part to 6.6 parts of zinc acetate, 6 parts to 40 parts of solvent, 0.1 part to 0.6 part of surfactant, by the original chosen
Material mixing after with monoethanolamine adjust pH value be 6 to 8 between i.e. obtain the present invention the swollen clay stabilizer of water-fastness contracting.
Here is the further optimization and/or improvements to one of foregoing invention technical scheme:
Above-mentioned oxidant I is ammonium persulfate;Or/and, oxidant II is ammonium persulfate;Or/and, polymer is molecular weight 8,000,000
To 12,000,000 polyacrylamide;Or/and, solvent is deionized water or ethanol solution.
Above-mentioned surfactant is anion surfactant.
Above-mentioned surfactant is dodecyl sodium sulfate.
The two of technical scheme are realized by following measures:A kind of water-fastness swollen clay stabilizer of contracting
Preparation method, is carried out as follows:The first step, first by 12/14 tertiary amines and concentration for 31% to 38% hydrochloric acid solution with
Mol ratio 1:1.5 are mixed into quaternary ammonium salt mother liquor, then the oxidant of addition quaternary ammonium salt mother liquor 0.07% to 0.12% into quaternary ammonium salt mother liquor
I, reaction 30min to 35min obtains mother liquor I under the conditions of temperature is 15 DEG C to 20 DEG C;
Second step, by hexamethylenetetramine and concentration for 36% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into six first
Urotropine hydrochloric acid mother liquor, then aluminium ion crosslinking agent is added into hexamethylenetetramine hydrochloric acid mother liquor, wherein in aluminium ion crosslinking agent
Aluminium ion accounts for the 0.1% to 1% of hexamethylenetetramine hydrochloric acid mother liquor, then selects the mode of gradient increased temperature to be reacted:First heat up
To 20 DEG C to 30 DEG C progress first set reactions, the first set reaction time be 30min to 35min, then be warming up to 45 DEG C to 55 DEG C and enter
The secondary response of row second, second reaction time be 30min to 35min, finally obtain mother liquor II;
3rd step, by weight meter choose I 19 parts to 39 parts of raw material mother liquor, II 9 parts to 29 parts of mother liquor, molecular weight be 300,000 to
500000 0.5 part to 5 parts of polyquaternium, II 0.1 parts to 1 part of oxidant, 0.01 part to 0.1 part of polymer, 1.7 parts of zirconium oxychloride
To 9.7 parts, 0.6 part to 6.6 parts of zinc acetate, 6 parts to 40 parts of solvent, 0.1 part to 0.6 part of surfactant, by the original chosen
Material mixing after with monoethanolamine adjust pH value be 6 to 8 between i.e. obtain the present invention the swollen clay stabilizer of water-fastness contracting.
Here is two further optimization and/or improvements to foregoing invention technical scheme:
Above-mentioned oxidant I is ammonium persulfate;Or/and, oxidant II is ammonium persulfate;Or/and, polymer is molecular weight 8,000,000
To 12,000,000 polyacrylamide;Or/and, solvent is deionized water or ethanol solution.
Above-mentioned surfactant is anion surfactant.
Above-mentioned surfactant is dodecyl sodium sulfate.
The present invention by compounding the need for synthesize certain density mother liquor, then compound the water-fastness contracting for obtaining the present invention
Swollen clay stabilizer, not only with the swollen performance that preferably contracts, while having preferable wash durability, preparation process is simple easily real
Apply, it is functional.
Embodiment
The present invention is not limited by following embodiments, can technique according to the invention scheme and actual conditions it is specific to determine
Embodiment.Various chemical reagent and chemical article are previously mentioned in the present invention unless otherwise specified, is known in existing technology
Public chemical reagent and chemical article;Percentage in the present invention is as being mass percent without specified otherwise;The present invention
In water as being running water or pure water without specified otherwise;It is that solvent is if the solution in the present invention is without specified otherwise
The aqueous solution of water, for example, hydrochloric acid solution is aqueous hydrochloric acid solution;Normal temperature in the present invention refers generally to 15 DEG C to 25 DEG C of temperature,
It is commonly defined as 25 DEG C.
With reference to embodiment, the invention will be further described:
Embodiment 1, the water-fastness swollen clay stabilizer of contracting is obtained by following preparation methods:The first step, first by 12/14 tertiary amines
With concentration for 31% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into quaternary ammonium salt mother liquor, then are added into quaternary ammonium salt mother liquor
The oxidant I of quaternary ammonium salt mother liquor 0.07% to 0.12%, reaction 30min to 35min is obtained under the conditions of temperature is 15 DEG C to 20 DEG C
Mother liquor I;
Second step, by hexamethylenetetramine and concentration for 36% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into six first
Urotropine hydrochloric acid mother liquor, then aluminium ion crosslinking agent is added into hexamethylenetetramine hydrochloric acid mother liquor, wherein in aluminium ion crosslinking agent
Aluminium ion accounts for the 0.1% to 1% of hexamethylenetetramine hydrochloric acid mother liquor, then selects the mode of gradient increased temperature to be reacted:First heat up
To 20 DEG C to 30 DEG C progress first set reactions, the first set reaction time be 30min to 35min, then be warming up to 45 DEG C to 55 DEG C and enter
The secondary response of row second, second reaction time be 30min to 35min, finally obtain mother liquor II;To avoid reaction insufficient, choosing
Select a point gradient increased temperature reaction.
It is 30 that 3rd step, by weight meter, which choose I 19 parts to 39 parts of raw material mother liquor, II 9 parts to 29 parts of mother liquor, molecular weight,
Ten thousand to 500,000 0.5 part to 5 parts of polyquaternium, II 0.1 parts to 1 part of oxidant, 0.01 part to 0.1 part of polymer, zirconium oxychloride
1.7 parts to 9.7 parts, 0.6 part to 6.6 parts of zinc acetate, 6 parts to 40 parts of solvent, 0.1 part to 0.6 part of surfactant, will choose
Raw material mixing after with monoethanolamine adjust pH value be 6 to 8 between i.e. obtain the present invention the swollen clay stabilizer of water-fastness contracting.
The present invention by first synthesizing certain density mother liquor, then compound obtain the present invention the swollen clay of water-fastness contracting it is steady
Determine agent, not only with the swollen performance that preferably contracts, while having preferable wash durability, preparation process is simply easily implemented, performance
Well.In the present invention cation inhibitor is used as from polyquaternium.
Embodiment 2, the water-fastness swollen clay stabilizer of contracting is obtained by following preparation methods:The first step, first by 12/14
Tertiary amine and concentration for 31% or 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into quaternary ammonium salt mother liquor, then into quaternary ammonium salt mother liquor
Quaternary ammonium salt mother liquor 0.07% or 0.12% oxidant I are added, reaction 30min or 35min is obtained under the conditions of temperature is 15 DEG C or 20 DEG C
To mother liquor I;
Second step, by hexamethylenetetramine and concentration for 36% or 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into six first
Urotropine hydrochloric acid mother liquor, then aluminium ion crosslinking agent is added into hexamethylenetetramine hydrochloric acid mother liquor, wherein in aluminium ion crosslinking agent
Aluminium ion accounts for the 0.1% or 1% of hexamethylenetetramine hydrochloric acid mother liquor, then selects the mode of gradient increased temperature to be reacted:First heat up
First set reactions are carried out to 20 DEG C or 30 DEG C, the first set reaction time is 30min or 35min, then are warming up to 45 DEG C or 55 DEG C to enter
The secondary response of row second, second of reaction time is 30min or 35min, finally obtains mother liquor II;To avoid reaction insufficient, choosing
Select a point gradient increased temperature reaction.
It is 30 that 3rd step, by weight meter, which choose I 19 parts or 39 parts of raw material mother liquor, II 9 parts or 29 parts of mother liquor, molecular weight,
Ten thousand or 500,000 0.5 part or 5 parts of polyquaternium, II 0.1 parts or 1 part of oxidant, 0.01 part or 0.1 part of polymer, zirconium oxychloride
1.7 parts or 9.7 parts, 0.6 part or 6.6 parts of zinc acetate, 6 parts or 40 parts of solvent, 0.1 part or 0.6 part of surfactant, will choose
Raw material mixing after with monoethanolamine adjust pH value be 6 or 8 i.e. obtain the present invention the swollen clay stabilizers of water-fastness contracting.
Embodiment 3, as the optimization of above-described embodiment, oxidant I is ammonium persulfate;Or/and, oxidant II is persulfuric acid
Ammonium;Or/and, polymer is the polyacrylamide of molecular weight 8,000,000 to 12,000,000;Or/and, solvent is that deionized water or ethanol are molten
Liquid.Ethanol solution is to obtain ethanol water after absolute ethyl alcohol and deionized water are mixed by any ratio;
Embodiment 4, as the optimization of above-described embodiment, surfactant is anion surfactant.
Embodiment 5, as the optimization of above-described embodiment, surfactant is dodecyl sodium sulfate.
Following contracting is carried out using the swollen clay stabilizer of water-fastness contracting obtained according to the above embodiment of the present invention respectively swollen
Benchmark test, test method is with reference to SY/T5971-2016《People's Republic of China's oil and gas industry standard》In " oil
7.4 in gas field fracture acidizing and water filling clay stabilizer method of evaluating performance ";Evaluation result is shown in Table 1, table 2, table 3 and table
4, the inventive samples in table are the swollen clay stabilizer of water-fastness contracting obtained according to the above embodiment of the present invention, comparative sample
1., control sample 2., control sample be 4. 3. the conventional use of medicament with the swollen performance of contracting in the prior art with control sample.
The water-fastness contracting obtained it can be seen from table 1, table 2, table 3 and the data of table 4 according to the above embodiment of the present invention is swollen viscous
Soil stabilizer either carries out liquid experiment or solid experiment indoors, or applied to scene, after first time washes just
The swollen performance that preferably contracts has been embodied, and after third time is washed, can further play its swollen performance of contracting, simultaneously
With preferable wash durability.Also, by the swollen clay stabilizer application of water-fastness contracting obtained according to the above embodiment of the present invention
When scene, after the injection of the scene of wind 33, falloff curve is gathered, pressure is steady after slowly declining, and injection situation is stable, later stage injection
Continuation it is good;After the injection of husky south scene, falloff curve is gathered, pressure is steady after slowly declining, and injection situation is stable, the later stage
The continuation of injection is good.
The conventional use of medicament with the swollen performance of contracting in the prior art it can be seen from table 1, table 2, table 3 and the data of table 4
Either carry out liquid experiment or solid experiment indoors, or applied to scene, after first time washes, the swollen performance that contracts without
Embody, after third time is washed, what is had has the swollen performance of less contracting, have still without any swollen performance of contracting, even if having
Washed by third time, with the swollen performance of less contracting, but its relative to primary sample it may be said that the swollen property that still do not contract
Can, and it is for the swollen clay stabilizer of water-fastness contracting of the present invention, the swollen performance of contracting embodied after the washing of its third time
Substantially well below the swollen performance of contracting of the swollen clay stabilizer of water-fastness contracting of the invention, while wash durability is poor.
Therefore, the swollen clay stabilizer of water-fastness contracting according to obtained by the above embodiment of the present invention not only has preferably
Contract swollen performance, while having preferable wash durability.
Above technical characteristic constitutes embodiments of the invention, and it has stronger adaptability and implementation result, can basis
The non-essential technical characteristic of increase and decrease is actually needed, to meet the demand of different situations.
Claims (10)
1. a kind of water-fastness swollen clay stabilizer of contracting, it is characterised in that obtain as follows:The first step, first by 12/14
Tertiary amine and concentration for 31% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into quaternary ammonium salt mother liquor, then into quaternary ammonium salt mother liquor
The oxidant I of quaternary ammonium salt mother liquor 0.07% to 0.12% is added, 30min to 35min is reacted under the conditions of temperature is 15 DEG C to 20 DEG C
Obtain mother liquor I;
Second step, by hexamethylenetetramine and concentration for 36% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into six first
Urotropine hydrochloric acid mother liquor, then aluminium ion crosslinking agent is added into hexamethylenetetramine hydrochloric acid mother liquor, wherein in aluminium ion crosslinking agent
Aluminium ion accounts for the 0.1% to 1% of hexamethylenetetramine hydrochloric acid mother liquor, then selects the mode of gradient increased temperature to be reacted:First heat up
To 20 DEG C to 30 DEG C progress first set reactions, the first set reaction time be 30min to 35min, then be warming up to 45 DEG C to 55 DEG C and enter
The secondary response of row second, second reaction time be 30min to 35min, finally obtain mother liquor II;
3rd step, by weight meter choose I 19 parts to 39 parts of raw material mother liquor, II 9 parts to 29 parts of mother liquor, molecular weight be 300,000 to
500000 0.5 part to 5 parts of polyquaternium, II 0.1 parts to 1 part of oxidant, 0.01 part to 0.1 part of polymer, 1.7 parts of zirconium oxychloride
To 9.7 parts, 0.6 part to 6.6 parts of zinc acetate, 6 parts to 40 parts of solvent, 0.1 part to 0.6 part of surfactant, by the original chosen
Material mixing after with monoethanolamine adjust pH value be 6 to 8 between i.e. obtain the present invention the swollen clay stabilizer of water-fastness contracting.
2. the water-fastness swollen clay stabilizer of contracting according to claim 1, it is characterised in that oxidant I is ammonium persulfate;Or/
It is ammonium persulfate with, oxidant II;Or/and, polymer is the polyacrylamide of molecular weight 8,000,000 to 12,000,000;Or/and, it is molten
Agent is deionized water or ethanol solution.
3. the water-fastness swollen clay stabilizer of contracting according to claim 1 or 2, it is characterised in that surfactant is anion
Surfactant.
4. the water-fastness swollen clay stabilizer of contracting according to claim 1 or 2, it is characterised in that surfactant is dodecane
Base sodium sulfonate.
5. the water-fastness swollen clay stabilizer of contracting according to claim 3, it is characterised in that surfactant is dodecyl
Sodium sulfonate.
6. a kind of preparation method of the water-fastness swollen clay stabilizer of contracting, it is characterised in that carry out as follows:The first step, first will
12/14 tertiary amines and concentration for 31% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into quaternary ammonium salt mother liquor, then to quaternary ammonium
The oxidant I of quaternary ammonium salt mother liquor 0.07% to 0.12% is added in salt mother liquor, 30min is reacted extremely under the conditions of temperature is 15 DEG C to 20 DEG C
35min obtains mother liquor I;
Second step, by hexamethylenetetramine and concentration for 36% to 38% hydrochloric acid solution with mol ratio 1:1.5 are mixed into six first
Urotropine hydrochloric acid mother liquor, then aluminium ion crosslinking agent is added into hexamethylenetetramine hydrochloric acid mother liquor, wherein in aluminium ion crosslinking agent
Aluminium ion accounts for the 0.1% to 1% of hexamethylenetetramine hydrochloric acid mother liquor, then selects the mode of gradient increased temperature to be reacted:First heat up
To 20 DEG C to 30 DEG C progress first set reactions, the first set reaction time be 30min to 35min, then be warming up to 45 DEG C to 55 DEG C and enter
The secondary response of row second, second reaction time be 30min to 35min, finally obtain mother liquor II;
3rd step, by weight meter choose I 19 parts to 39 parts of raw material mother liquor, II 9 parts to 29 parts of mother liquor, molecular weight be 300,000 to
500000 0.5 part to 5 parts of polyquaternium, II 0.1 parts to 1 part of oxidant, 0.01 part to 0.1 part of polymer, 1.7 parts of zirconium oxychloride
To 9.7 parts, 0.6 part to 6.6 parts of zinc acetate, 6 parts to 40 parts of solvent, 0.1 part to 0.6 part of surfactant, by the original chosen
Material mixing after with monoethanolamine adjust pH value be 6 to 8 between i.e. obtain the present invention the swollen clay stabilizer of water-fastness contracting.
7. the preparation method of the swollen clay stabilizer of water-fastness contracting according to claim 6, it is characterised in that oxidant I was
Ammonium sulfate;Or/and, oxidant II is ammonium persulfate;Or/and, polymer is the polyacrylamide of molecular weight 8,000,000 to 12,000,000
Amine;Or/and, solvent is deionized water or ethanol solution.
8. the preparation method of the swollen clay stabilizer of water-fastness contracting according to claim 6 or 7, it is characterised in that surface-active
Agent is anion surfactant.
9. the preparation method of the swollen clay stabilizer of water-fastness contracting according to claim 6 or 7, it is characterised in that surface-active
Agent is dodecyl sodium sulfate.
10. the preparation method of the water-fastness swollen clay stabilizer of contracting according to claim 8, it is characterised in that surfactant
For dodecyl sodium sulfate.
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CN202211113629.8A CN115404054A (en) | 2017-07-28 | 2017-07-28 | Washing-resistant shrinkage-expansion clay stabilizer and preparation method and application thereof |
CN201710635559.5A CN107325795A (en) | 2017-07-28 | 2017-07-28 | Water-fastness swollen clay stabilizer of contracting and preparation method thereof |
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CN201710635559.5A Pending CN107325795A (en) | 2017-07-28 | 2017-07-28 | Water-fastness swollen clay stabilizer of contracting and preparation method thereof |
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CN104418984A (en) * | 2013-09-04 | 2015-03-18 | 中国石油化工股份有限公司 | High-temperature resistant clay stabilizer and preparation method thereof |
CN104588199A (en) * | 2015-01-19 | 2015-05-06 | 中国矿业大学 | Method for inhibiting argillization in coal washing and selecting process |
CN104910879A (en) * | 2015-04-09 | 2015-09-16 | 陕西海默油田服务有限公司 | Anti-sloughing drilling fluid and well slough preventing method |
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CN105623636B (en) * | 2014-10-27 | 2019-05-07 | 中国石油天然气股份有限公司 | Swelling-resistant shrinking and swelling agent, preparation method and its application |
CN106947440B (en) * | 2017-03-30 | 2022-03-29 | 山东滨州昱诚化工科技有限公司 | Temperature-resistant salt-resistant anti-swelling clay stabilizer and preparation method thereof |
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- 2017-07-28 CN CN202211113629.8A patent/CN115404054A/en active Pending
- 2017-07-28 CN CN201710635559.5A patent/CN107325795A/en active Pending
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CN104418984A (en) * | 2013-09-04 | 2015-03-18 | 中国石油化工股份有限公司 | High-temperature resistant clay stabilizer and preparation method thereof |
CN104588199A (en) * | 2015-01-19 | 2015-05-06 | 中国矿业大学 | Method for inhibiting argillization in coal washing and selecting process |
CN104910879A (en) * | 2015-04-09 | 2015-09-16 | 陕西海默油田服务有限公司 | Anti-sloughing drilling fluid and well slough preventing method |
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Application publication date: 20171107 |