CN105670575A - Shale inhibitor and preparation method thereof - Google Patents
Shale inhibitor and preparation method thereof Download PDFInfo
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- CN105670575A CN105670575A CN201610017644.0A CN201610017644A CN105670575A CN 105670575 A CN105670575 A CN 105670575A CN 201610017644 A CN201610017644 A CN 201610017644A CN 105670575 A CN105670575 A CN 105670575A
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- control agent
- shale
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- shale control
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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
- C09K8/035—Organic additives
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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
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- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The invention discloses a shale inhibitor. The shale inhibitor is prepared from 15-35% by mass of poly(diallyldimethylammonium chloride), 10-25% by mass of polyether amine, 10-25% by mass of oxalic acid, 15-35% by mass of choline chloride and 15-40% by mass of water. Polyether amine, oxalic acid, poly(diallyldimethylammonium chloride) and choline chloride undergo a reaction to produce a polyamine shale inhibitor. The polyamine shale inhibitor can effectively inhibit shale hydration expansion, has low toxicity, a small ammonia smell, high heat stability and good compatibility with other treatment agents and is an amine shale inhibitor with most potential for development at present. An experiment result shows that the shale inhibitor has a roll recovery rate of 87.6% or more, a volume expansion ratio less than 11.0% and a water loss less than 29.6mL.
Description
Technical field
The present invention relates to field of oil drilling, particularly relate to a kind of shale control agent and preparation method thereof.
Background technology
Mud shale stratum clay ratio contained by it is high, easy aquation, bring great negative effect to drillng operation, drilling process often occurs a series of down hole problems such as borehole well instability, caliper expansion, bit freezing, moment of torsion and resistance increase, adds drilling well difficulty. Therefore bore when meeting mud shale stratum and must improve the drilling fluid inhibition to mud shale, reduce the incidence rate of down hole problem to greatest extent. Conventional shale control agent mainly has polymer class, inorganic salts, Colophonium class and humic-acid kind etc.; these shale control agents are all individually present some shortcomings; as Colophonium class is unfavorable for protection environment; silicate can make system rheological characteristic be difficult to regulate and control, and glucosides class, polyethylene glycols can not solve the drilling problem of activity mud shale.
Summary of the invention
In view of this, the present invention proposes a kind of shale control agent and preparation method thereof, and this shale control agent can solve the problem that the drilling problem of mud shale bottom.
The technical scheme is that and be achieved in that:
A kind of shale control agent, forms including the preparation of raw material with mass percent:
Preferably, form including the preparation of raw material with mass percent:
Preferably, described water is pure water or ultra-pure water.
The preparation method that present invention also offers a kind of shale control agent, it is characterised in that comprise the following steps:
1) in reactor, add water and polyetheramine, obtain the first mixed liquor;
2) to step 1) described first mixed liquor that obtains adds oxalic acid, and control the temperature in reactor, obtain the second mixed solution;
3) to step 2) described second mixed solution that obtains adds PDDA and choline chloride, namely stirring reaction obtains polyamine class shale control agent.
Preferably, step 2) described in temperature in reactor be 50～100 DEG C, the response time is 2～4h.
Preferably, step 3) particularly as follows: to step 2) described second mixed solution that obtains adds PDDA and choline chloride, continuing stirring and maintain reactor temperature, the response time is 0.5～2h, namely prepares polyamine class shale control agent.
The invention have the benefit that
In the present invention, adopt the polyamine class shale control agent that polyetheramine, oxalic acid, PDDA and choline chloride are obtained by reacting, shale hydration can be effectively suppressed to expand, and there is low toxicity, low ammonia odor, heat stability height and the feature good with other inorganic agent compatibilities, it is the most potential current amine shale control agent.Test result indicate that, the rolling response rate of shale control agent provided by the invention is more than 87.6%, and cubical expansivity is lower than 11.0%, and dehydration is lower than 29.6mL.
Detailed description of the invention
The invention discloses a kind of shale control agent and preparation method thereof, those skilled in the art can use for reference present disclosure, is suitably modified technological parameter and realizes. Special needs to be pointed out is, described similar replacement and change apparent to those skilled in the art, they are considered as including in the present invention. The method of the present invention and quoting is described already by preferred embodiment, method described herein and application substantially can be modified or suitably change and combination by related personnel in without departing from present invention, spirit and scope, realize and apply the technology of the present invention.
A kind of shale control agent, forms including the preparation of raw material with mass percent:
In the present invention, PDDA plays gelatification. Wherein, the mass percent of PDDA is 15～35%. In an embodiment of the present invention, the mass percent of PDDA is 20～30%; In other enforcements of the present invention, the mass percent of PDDA is 23～27%.
In the present invention, polyetheramine is as aminated compounds; The mass percent of polyetheramine is 10～25%. In an embodiment of the present invention, the mass percent of polyetheramine is 15～20%; In other embodiments, the mass percent of polyetheramine is 17～18%.
In the present invention, oxalic acid is as acid compounds, for reacting generation shale control agent with above-mentioned aminated compounds. The mass percent of its mesoxalic acid is 10～25%. In an embodiment of the present invention, the mass percent of oxalic acid is 12～20%; In other embodiments, the mass percent of oxalic acid is 14～18%.
In the present invention, choline chloride plays the effect suppressing shale expansion. Wherein, the mass percent of choline chloride is 15～35. In an embodiment of the present invention, the mass percent of choline chloride is 20～30%; In other embodiments, the mass percent of choline chloride is 24～26%.
In the present invention, water plays the effect of diluent. Wherein, the mass percent of water is 15～40%. In an embodiment of the present invention, the mass percent of water is 20～30%.
In an embodiment of the present invention, water is pure water or ultra-pure water.
The restriction that the present invention is not special to the source of all raw materials, for commercially available.
The preparation method that the invention also discloses a kind of shale control agent, comprises the following steps:
1) in reactor, add water and polyetheramine, obtain the first mixed liquor;
2) to step 1) described first mixed liquor that obtains adds oxalic acid, and control the temperature in reactor, obtain the second mixed solution;
3) to step 2) described second mixed solution that obtains adds PDDA and choline chloride, namely stirring reaction obtains polyamine class shale control agent.
The source of all raw materials of the present invention is not particularly limited, for commercially available.
Wherein, water, polyetheramine, oxalic acid, PDDA and choline chloride are all same as above, do not repeat them here.
In the present invention, polyetheramine first reacts with oxalic acid, the polyamine class shale control agent being obtained by reacting with PDDA and choline chloride again, shale hydration can be effectively suppressed to expand, and there is low toxicity, low ammonia odor, heat stability height and the feature good with other inorganic agent compatibilities, it is the most potential current amine shale control agent;Improve inhibition further and reduce toxicity, it is achieved the developing direction that " green " drilling fluid system will be amine inhibitor and drilling fluid system thereof.
In an embodiment of the present invention, polyetheramine and oxalic acid reaction temperature are 50～100 DEG C, and the response time is 2～4h; In other embodiments, polyetheramine and oxalic acid reaction temperature are 70～80 DEG C.
In an embodiment of the present invention, step 3) specifically, the second mixed solution adds PDDA and choline chloride, to continue stirring and maintain reactor temperature, the response time is 0.5～2h, namely prepares polyamine class shale control agent.
Raw material used in shale control agent provided by the invention and preparation method thereof all can be buied by market.
In order to be further appreciated by the present invention, below in conjunction with embodiment, substrate provided by the invention and preparation method thereof being illustrated, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Take 25g pure water, 15g polyetheramine joins in reactor, is uniformly mixing to obtain the first mixture; In the first mixture, add 15g oxalic acid, at 75 DEG C, react 3h, obtain the second mixed solution; In the second mixed solution, add 15g PDDA and 30g choline chloride, keep the temperature in reactor, react 1.5h, namely obtain polyamine class shale control agent.
Embodiment 2
Take 18g ultra-pure water and 10g polyetheramine joins in reactor, be uniformly mixing to obtain the first mixture; In the first mixture, add 12g oxalic acid, at 80 DEG C, react 4h, obtain the second mixed solution; In the second mixed solution, add 25g PDDA and 35g choline chloride, keep the temperature in reactor, react 2h, namely obtain polyamine class shale control agent.
Embodiment 3
Take 15g pure water and 20g polyetheramine joins in reactor, be uniformly mixing to obtain the first mixture; In the first mixture, add 20g oxalic acid, at 75 DEG C, react 3h, obtain the second mixed solution; In the second mixed solution, add 30g PDDA and 15g choline chloride, keep the temperature in reactor, react 1.5h, namely obtain polyamine class shale control agent.
Embodiment 4
Take 20g ultra-pure water and 25g polyetheramine joins in reactor, be uniformly mixing to obtain the first mixture; In the first mixture, add 10g oxalic acid, at 75 DEG C, react 3h, obtain the second mixed solution; In the second mixed solution, add 25g PDDA and 20g choline chloride, keep the temperature in reactor, react 1.5h, namely obtain polyamine class shale control agent.
Embodiment 5
Take 30g pure water and 10g polyetheramine joins in reactor, be uniformly mixing to obtain the first mixture; In the first mixture, add 20g oxalic acid, at 100 DEG C, react 2h, obtain the second mixed solution; In the second mixed solution, add 15g PDDA and 25g choline chloride, keep the temperature in reactor, react 1h, namely obtain polyamine class shale control agent.
Embodiment 6
Take 40g ultra-pure water and 12g polyetheramine joins in reactor, be uniformly mixing to obtain the first mixture; In the first mixture, add 13g oxalic acid, at 50 DEG C, react 4h, obtain the second mixed solution; In the second mixed solution, add 20g PDDA and 15g choline chloride, keep the temperature in reactor, react 1.5h, namely obtain polyamine class shale control agent.
Embodiment 7
Take 20g pure water and 16g polyetheramine joins in reactor, be uniformly mixing to obtain the first mixture; In the first mixture, add 25g oxalic acid, at 75 DEG C, react 3h, obtain the second mixed solution; In the second mixed solution, add 15g PDDA and 24g choline chloride, keep the temperature in reactor, react 2h, namely obtain polyamine class shale control agent.
Performance evaluation
1) response rate evaluation is rolled
1.1 roll response rate evaluation methodology
Take the base slurry 350m containing sodium bentonite 7% in high speed cup, high-speed stirred 15～20min after addition polyamine class shale control agent, make inorganic agent fully dispersed, it is then introduced in roller furnace ageing can, stir after adding 6～120 order drilling cuttings 30g, after rolling 6h at 60 DEG C, go out not scattered drilling cuttings with 40 mesh screen. The dry W that is weighed as, calculating rolls the response rate (W/30 × 100%).
1.2 roll determination of recovery rates
Above-described embodiment 1～7 by volume expansion rate evaluation methodology being evaluated, result is shown in Table 1.
2) volumetric expansion evaluation
2.1 volumetric expansion evaluation methodologys
Take three centrifuge tubes, the first centrifuge tube is contained 0.5g sodium bentonite, 10ml kerosene; Second centrifuge tube is contained 0.5g sodium bentonite, 10ml water; 3rd centrifuge tube is contained 0.5g sodium bentonite, 10ml polyamine class shale control agent. After aquation 2h, with centrifuge high speed centrifugation 20min, measuring bentonite volume in kerosene is V0, in water, bentonitic volume is V1, in polyamine class shale control agent, bentonite volume is V2. Calculate anti-expansion rate ρ=(V1-V2)/(V1-V0) × 100%.
2.2 cubical expansivities measure
Above-described embodiment 1～7 by volume expansion rate evaluation methodology being evaluated, result is shown in Table 1.
3) dehydration evaluation
3.1 dehydration evaluation methodologys
Measure 400mL water, be added thereto to 16g sodium bentonite and 0.8g natrium carbonicum calcinatum, high-speed stirred 20min under 10000r/min, be a base slurry, place 24h standby; Take a base slurry, it is added thereto to 6g polyamine sample, under 10000r/min after high-speed stirred 20min, aging 16h at 180 DEG C, take out after cooling, under 10000r/min after high-speed stirred 5min, by by the API filtration (room temperature/0.69MPa) after the method test high temperature ageing of 7.2 joints in GB/T16783.1-2006.
1.2 dehydrations measure
Being evaluated by dehydration evaluation methodology by above-described embodiment 1～7, result is shown in Table 1.
Table 1 embodiment 1～7 rolls the response rate, cubical expansivity and dehydration measurement result
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (6)
1. a shale control agent, it is characterised in that include forming with the preparation of raw material of mass percent:
2. shale control agent as claimed in claim 1, it is characterised in that include forming with the preparation of raw material of mass percent:
3. shale control agent as claimed in claim 1, it is characterised in that described water is pure water or ultra-pure water.
4. the preparation method of the shale control agent as described in any one of claims 1 to 3, it is characterised in that comprise the following steps:
1) in reactor, add water and polyetheramine, obtain the first mixed liquor;
2) to step 1) described first mixed liquor that obtains adds oxalic acid, and control the temperature in reactor, obtain the second mixed solution;
3) to step 2) described second mixed solution that obtains adds PDDA and choline chloride, namely stirring reaction obtains polyamine class shale control agent.
5. preparation method as claimed in claim 4, it is characterised in that step 2) described in temperature in reactor be 50～100 DEG C, the response time is 2～4h.
6. preparation method as claimed in claim 4, it is characterized in that, step 3) particularly as follows: to step 2) described second mixed solution that obtains adds PDDA and choline chloride, continue stirring and maintain reactor temperature, response time is 0.5～2h, namely prepares polyamine class shale control agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610017644.0A CN105670575A (en) | 2016-01-12 | 2016-01-12 | Shale inhibitor and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610017644.0A CN105670575A (en) | 2016-01-12 | 2016-01-12 | Shale inhibitor and preparation method thereof |
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| CN105670575A true CN105670575A (en) | 2016-06-15 |
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| CN201610017644.0A Pending CN105670575A (en) | 2016-01-12 | 2016-01-12 | Shale inhibitor and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106497528A (en) * | 2016-11-03 | 2017-03-15 | 中国石油大学(华东) | A kind of shale-control agent for drilling fluid and preparation method thereof |
| CN108728058A (en) * | 2018-06-29 | 2018-11-02 | 长江大学 | A kind of drilling fluid inhibitor and its application |
| CN109868130A (en) * | 2019-03-01 | 2019-06-11 | 北京瓜尔润科技股份有限公司 | A kind of slippery water fracturing fluid |
| CN110982496A (en) * | 2019-12-24 | 2020-04-10 | 中国海洋石油集团有限公司 | Oil-based drilling fluid, preparation method thereof and preparation method of anti-settling stabilizer |
-
2016
- 2016-01-12 CN CN201610017644.0A patent/CN105670575A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106497528A (en) * | 2016-11-03 | 2017-03-15 | 中国石油大学(华东) | A kind of shale-control agent for drilling fluid and preparation method thereof |
| CN106497528B (en) * | 2016-11-03 | 2018-06-26 | 中国石油大学(华东) | A kind of shale-control agent for drilling fluid and preparation method thereof |
| CN108728058A (en) * | 2018-06-29 | 2018-11-02 | 长江大学 | A kind of drilling fluid inhibitor and its application |
| CN109868130A (en) * | 2019-03-01 | 2019-06-11 | 北京瓜尔润科技股份有限公司 | A kind of slippery water fracturing fluid |
| CN109868130B (en) * | 2019-03-01 | 2021-06-22 | 北京瓜尔润科技股份有限公司 | Slickwater fracturing fluid |
| CN110982496A (en) * | 2019-12-24 | 2020-04-10 | 中国海洋石油集团有限公司 | Oil-based drilling fluid, preparation method thereof and preparation method of anti-settling stabilizer |
| CN110982496B (en) * | 2019-12-24 | 2022-04-08 | 中国海洋石油集团有限公司 | Oil-based drilling fluid, preparation method thereof and preparation method of anti-settling stabilizer |
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Application publication date: 20160615 |
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