CN109694697A - A kind of drilling fluid polyamine shale inhibitor and preparation method thereof and drilling fluid - Google Patents
A kind of drilling fluid polyamine shale inhibitor and preparation method thereof and drilling fluid Download PDFInfo
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- CN109694697A CN109694697A CN201710992767.0A CN201710992767A CN109694697A CN 109694697 A CN109694697 A CN 109694697A CN 201710992767 A CN201710992767 A CN 201710992767A CN 109694697 A CN109694697 A CN 109694697A
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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
- 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
- C09K2208/34—Lubricant additives
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Abstract
The present invention provides a kind of drilling fluid preparation methods of polyamine shale inhibitor, comprising: reacts chloro epoxides, acidic catalyst, polyethylene polyamine, ethanol amine, thionyl chloride and ethylenediamine, obtains drilling fluid polyamine shale inhibitor.The present invention prepares polyamine shale inhibitor using specific raw material, and thionyl chloride is especially added in prepared composition, and the drilling fluid being prepared is made to have preferable shale inhibition and clay stability with polyamine shale inhibitor.Moreover, the polyamine shale inhibitor that method provided by the invention is prepared also has preferable greasy property and compatibility, and no biotoxicity.Polyamine shale inhibitor provided by the invention can be applied in drilling fluid, suitable for requiring higher strong retraction mud shale, containing caving grounds and shale gas Horizontal Well Drilling well constructions such as mud stone.The present invention also provides a kind of drilling fluid polyamine shale inhibitors.
Description
Technical field
The present invention relates to additive for drilling fluid technical field more particularly to a kind of drilling fluid polyamine shale inhibitor and
Preparation method and drilling fluid.
Background technique
Polyamine refers to the polymer in constitutional repeating unit containing amido, and polyamine in drilling fluid as mud shale for inhibiting
Agent, rejection are better than potassium chloride, and polyamine can enter clay interlayer and form monolayer adsorption, while generate with clay crystal layer surface
Hydrogen bond action.The main function mechanism of polyamine potent inhibitor are as follows: polyamine partially dissociates the ammonium cation of formation in the solution, leads to
It crosses in electrostatic interaction with clay surface negative charge, reduces clay aquation repulsion；Polyamine and clay crystal layer surface form hydrogen bond simultaneously
Strengthen absorption, clay lamella is bound together by both electrostatic attraction and hydrogen bond collective effect, side by side extruding part Inter layer adsorption
Water weakens clay aquation；Polyamine is adsorbed on after clay surface, is enhanced clay surface hydrophobic, is prevented the entrance of hydrone, into
One step inhibits clay hydration swelling.Therefore, polyamine inhibitor shows excellent rejection.Polyamine inhibition is potent persistently,
Be conducive to wellbore stability and reservoir protection, can be used separately as drilling fluid inhibitor, anti-sloughing agent or clay stabilizer, it can also
To form polyamine drilling fluid system.
Polyamine shale inhibitor in the prior art is mainly to be formed to have certain three-dimensional-structure by cross-linked polymeric
It is crosslinked amine based polymer, reacts violent, not easy to control, and the caving control performance and compatibility for the polyamine being prepared are also
It is to be improved, to better meet the use demand of drilling fluid.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of drilling fluid polyamine shale inhibitors and preparation method thereof
And drilling fluid, drilling fluid provided by the invention have preferable caving control performance and compatibility with polyamine shale inhibitor
Energy.
The present invention provides a kind of drilling fluid preparation methods of polyamine shale inhibitor, comprising:
Chloro epoxides, acidic catalyst, polyethylene polyamine, ethanol amine, thionyl chloride and ethylenediamine are reacted,
Obtain drilling fluid polyamine shale inhibitor.
In the present invention, the matter of chloro epoxides, acidic catalyst, organic amine, ethanol amine, thionyl chloride and ethylenediamine
Amount is than being preferably 10:(30~60): (10~20): (5~15): (0.8~1.2): (10~20).
In the present invention, drilling fluid polyamine shale inhibitor preparation method preferably specifically includes the following steps:
(1) chloro epoxides is reacted under acidic catalyst catalysis, obtains chloro glycol；
(2) the pure and mild polyethylene polyamine of chloro two is reacted, obtains the first intermediate product；
(3) the first intermediate product, ethanol amine and thionyl chloride are reacted, obtains the second intermediate product；
(4) the second intermediate product and ethylenediamine are reacted, obtains drilling fluid polyamine shale inhibitor.
In the present invention, in step (1), chloro epoxides preferably includes epoxychloropropane or 1,2- epoxy chloro fourth
Alkane；Acidic catalyst is preferably hydrochloric acid, sulfuric acid, phosphoric acid, tartaric acid, oxalic acid, p-methyl benzenesulfonic acid, dodecyl benzene sulfonic acid, amino
Sulfonic acid or phosphotungstic acid.In the present invention, reaction temperature is preferably 85~105 DEG C in step (1), and the reaction time is preferably 0.5~
2.0h。
In the present invention, polyethylene polyamine preferably includes diethylenetriamine, triethylene tetramine, four ethylene five in step (2)
Amine or pentaethylene hexamine；Reaction temperature in step (2) is preferably 45~60 DEG C, more preferably 1.5~3.0h.
In the present invention, the reaction temperature in step (3) is preferably 80~95 DEG C, and the time of reaction is preferably 0.5~
2.0h。
In the present invention, the reaction temperature in step (4) is preferably 45~60 DEG C, and the reaction time is preferably 1.5~3.0h.
The present invention provides a kind of drilling fluid polyamine shale inhibitors, have structure shown in Formulas I:
In Formulas I, it be 1~4, o is 1~2 that m, which is 1~2, n,.
In the present invention, drilling fluid is preferably 378~550 with the number-average molecular weight of polyamine shale inhibitor.
The present invention provides a kind of drilling fluids, use including the drilling fluid that method described in above-mentioned technical proposal is prepared poly-
Amine shale inhibitor；Or the polyamine shale inhibitor of drilling fluid described in above-mentioned technical proposal.
The present invention is not particularly limited the ingredient of drilling fluid, since drilling fluid provided by the invention polyamine mud shale presses down
Preparation has good compatibility, and conventional water-base drilling fluid, such as saturated salt-water drilling fluid, without native phase drilling fluid, low solid
Phase-polymerization object drilling fluid, polysulfonated potassium drilling fluid etc. can be carried out the compounding of arbitrary proportion.
Compared with prior art, the present invention uses specified raw material, the drilling fluid being prepared particularly with the addition of thionyl chloride
Have preferable shale inhibition can be with clay stability with polyamine shale inhibitor.Moreover, method provided by the invention
The drilling fluid being prepared polyamine shale inhibitor has preferable greasy property and compatibility, and inanimate object poison
Property.In addition, the preparation method simple process of polyamine shale inhibitor provided by the invention, reaction condition is mild, convenient for operation.
Polyamine shale inhibitor provided by the invention is added in drilling fluid can make drilling fluid have preferable shale
Rejection, clay stability, greasy property and compatibility make drilling fluid be suitable for requiring higher strong retraction mud page
Rock contains caving grounds and the shale gas Horizontal Well Drilling well constructions such as mud stone.
The experimental results showed that the drilling fluid polyamine shale inhibitor provided by the invention that mass concentration is 1% is water-soluble
The shale primary recovery > 96% of liquid, shale relative recovery > 99%, clay relative inhibition > 97%.Mass concentration is
The extreme boundary lubrication coefficient < 0.08, EC of 1% drilling fluid provided by the invention polyamine shale inhibitor aqueous solution50Value >
480000mg/L.Drilling fluid polyamine shale inhibitor provided by the invention and conventional water-base drilling fluid can be multiple with arbitrary proportion
With not influencing rheological property.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff it is improved or retouching all other example, shall fall within the protection scope of the present invention.
The drilling fluid that the present invention is prepared is configured to the polyamine mud that mass concentration is 1% with polyamine shale inhibitor
Shale control agent aqueous solution, at 150 DEG C high temperature roll 16 hours, by the following method, test its shale primary recovery and
Shale relative recovery:
By above-mentioned mass concentration be 1% polyamine shale inhibitor aqueous solution under 7000 revs/min of speed high-speed stirring
After mixing 5min, pour into spare in ageing can；The landwaste of 2.0mm~5.0mm dry 4h at 103 DEG C is taken, room temperature is down to；It weighs
G0The polyamine shale inhibitor aqueous solution that g landwaste is put into ageing can and above-mentioned mass concentration is 1% rolls 16h at 150 DEG C,
It is taken out after cooling, sieves recycling landwaste with aperture 0.42mm, the dry 4h at 103 DEG C is down to room temperature and weighs recycling landwaste quality note
For G1；Then overweight recycling landwaste will have been claimed to be put into clear water at 150 DEG C and has rolled 16h, taken out after cooling, use aperture
0.42mm sieve recycling landwaste, the dry 4h at 103 DEG C are cooled to room temperature weighing recycling landwaste quality, are denoted as G2；According to following
Formula calculates shale primary recovery, shale secondary returning yield and shale relative recovery:
Shale primary recovery=G1/G0× 100%；
Shale secondary returning yield=G2/G0× 100%；
Shale relative recovery=shale secondary returning yield/shale primary recovery × 100%；
Clay relative inhibition is tested by the following method, method particularly includes:
Accurate 2 parts of distilled water for measuring 350mL, are put into height and stir in cup, and the anhydrous carbon of 1.75g is added in portion thereto
Sour sodium is to distill the polyamine shale inhibitor that the above-mentioned mass concentration of water quality 1.5% is 1% to quality is added in another
The natrium carbonicum calcinatum of aqueous solution and 1.75g dissolves it all；
The calcium bentonite for weighing 35g is added high stirring cup high speed stirring 10min, is fitted into high temperature aging tank, in 150
DEG C high temperature rolls 16h；Room temperature is down in taking-up；
Above-mentioned calcium Peng Run soil is mixed with the above-mentioned distilled water containing natrium carbonicum calcinatum, obtains the first mixed liquor；It will be above-mentioned
Calcium bentonite is mixed with the above-mentioned distilled water containing polyamine shale inhibitor aqueous solution, obtains the second mixed liquor；By described
One mixed liquor and the second mixed liquor stir 5min with high-speed mixer respectively, its viscosity are tested using rotational viscometer, under
It states formula and calculates clay relative inhibition:
In formula:
B-clay relative inhibition, %；
Stablize reading when Ф-the first mixed liquor rotary viscosity metering rotating speed is 100r/min；
Ф1Stablize reading when-the second mixed liquor rotary viscosity metering rotating speed is 100r/min.
By the following method, the polyamine shale inhibitor aqueous solution that above-mentioned mass concentration is 1% is tested at room temperature
Extreme boundary lubrication coefficient:
Using the extreme boundary lubrication instrument for the EP model that Zhengzhou north and south Instrument Design Co., Ltd provides, instrument is set in 300r/
15min is operated under min, then adjusting revolving speed is 60r/min；
Sliding block in instrument is immersed in the polyamine shale inhibitor aqueous solution that above-mentioned mass concentration is 1%, adjusts torsion
Spanner value is 16.95N/m, apparatus working 5min, and it is sliding to read the polyamine shale inhibitor aqueous solution soaking that mass concentration is 1%
The numerical value shown on instrument when block, extreme boundary lubrication coefficient calculation formula are as follows:
In above formula: K is extreme boundary lubrication coefficient；
X be mass concentration be 1% polyamine shale inhibitor aqueous solution soaking sliding block provided by the invention when instrument on
The numerical value of display.
The EC for the polyamine shale inhibitor aqueous solution provided by the invention that mass concentration is 1%50Value > 480000mg/L.
The conventional water-base drilling fluid of drilling fluid polyamine shale inhibitor provided by the invention and scene includes saturated brine
Drilling fluid can compound in any proportion without native phase drilling fluid, low solids polymer drilling fluid, polysulfonated potassium drilling fluid, have compared with
Good compatibility.
Raw material used in following embodiment of the present invention is commercial goods.
Embodiment 1
10g epoxychloropropane is reacted under 30g hydrochloric acid catalysis, 0.5h is reacted at 85 DEG C, obtains chloro glycol；It will
The pure and mild 10g ethylenediamine of above-mentioned chloro two is reacted, and is reacted 1.5h at 45 DEG C, is obtained intermediate product 1；By intermediate product 1,5g second
Hydramine is reacted with 0.8g thionyl chloride, reacts 0.5h at 80 DEG C, obtains intermediate product 2, intermediate product 2 again with 10g second two
Amine reacts, and reacts 1.5h at 45 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 94.18%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 1 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 1 is prepared has Formulas I structure, and in Formulas I, m takes 1, n to take 0, o
Take 1.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 1 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1, and table 1 is the embodiment of the present invention and the drilling fluid that comparative example is prepared
With polyamine shale inhibitor the performance test results.
Embodiment 2
10g epoxychloropropane is reacted under 35g sulfuric acid catalysis, 1.0h is reacted at 90 DEG C, obtains chloro glycol；It will
The pure and mild 15g diethylenetriamine of above-mentioned chloro two is reacted, and is reacted 2.0h at 50 DEG C, is obtained intermediate product 1；By intermediate product 1,
10g ethanol amine is reacted with 1.0g thionyl chloride, reacts 1.0h at 90 DEG C, obtains intermediate product 2, intermediate product 2 again with 15g
Reacting ethylenediamine reacts 2.0h at 50 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 95.42%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 2 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 2 is prepared has Formulas I structure, and in Formulas I, m takes 1, n to take 1, o
Take 1.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 2 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 3
10g epoxy chlorobutane is reacted under 40g phosphoric acid catalyzed, 1.5h is reacted at 95 DEG C, obtains chloro glycol；It will
The pure and mild 20g triethylene tetramine of above-mentioned chloro two is reacted, and is reacted 2.5h at 55 DEG C, is obtained intermediate product 1；By intermediate product 1,
15g ethanol amine is reacted with 1.2g thionyl chloride, reacts 1.5h at 95 DEG C, obtains intermediate product 2, intermediate product 2 again with 20g
Reacting ethylenediamine reacts 2.5h at 55 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 96.12%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 3 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 3 is prepared has Formulas I structure, and in Formulas I, m takes 2, n to take 2, o
Take 2.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 3 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 4
10g epoxychloropropane is reacted under 45g winestone acid catalysis, 2.0h is reacted at 105 DEG C, obtains chloro two
Alcohol；The pure and mild 20g tetraethylenepentamine of above-mentioned chloro two is reacted, 3.0h is reacted at 60 DEG C, obtains intermediate product 1；It will be intermediate
Product 1,15g ethanol amine are reacted with 1.2g thionyl chloride, react 2.0h at 95 DEG C, obtain intermediate product 2, intermediate product 2
Again with 20g reacting ethylenediamine, 3.0h is reacted at 60 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 96.32%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 4 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 4 is prepared has Formulas I structure, and in Formulas I, m takes 1, n to take 3, o
Take 1.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 4 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 5
10g epoxychloropropane is reacted under 60g Catalyzed by Oxalic Acid, 2.0h is reacted at 105 DEG C, obtains chloro glycol；
The pure and mild 20g pentaethylene hexamine of above-mentioned chloro two is reacted, 3.0h is reacted at 60 DEG C, obtains intermediate product 1；By intermediate product
1,15g ethanol amine is reacted with 1.2g thionyl chloride, reacts 2.0h at 95 DEG C, obtains intermediate product 2, intermediate product 2 again with
20g reacting ethylenediamine reacts 3.0h at 60 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 96.37%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 5 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 5 is prepared has Formulas I structure, and in Formulas I, m takes 1, n to take 4, o
Take 1.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 5 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 6
10g epoxy chlorobutane is reacted under 60g Catalyzed by p-Toluenesulfonic Acid, 2.0h is reacted at 105 DEG C, obtains chloro
Glycol；The pure and mild 20g pentaethylene hexamine of above-mentioned chloro two is reacted, 3.0h is reacted at 60 DEG C, obtains intermediate product 1；Will in
Between product 1,15g ethanol amine reacted with 1.2g thionyl chloride, react 2.0h at 95 DEG C, obtain intermediate product 2, intermediate product
2, again with 20g reacting ethylenediamine, react 3.0h at 60 DEG C, obtain drilling fluid polyamine shale inhibitor.Yield is 96.44%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 6 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 6 is prepared has Formulas I structure, and in Formulas I, m takes 2, n to take 4, o
Take 2.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 6 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 7
10g epoxy chlorobutane is reacted under the catalysis of 60g dodecyl benzene sulfonic acid, 2.0h is reacted at 105 DEG C, obtains
Chloro glycol；The pure and mild 20g pentaethylene hexamine of above-mentioned chloro two is reacted, 3.0h is reacted at 60 DEG C, obtains intermediate product 1；
Intermediate product 1,15g ethanol amine are reacted with 1.2g thionyl chloride, 2.0h is reacted at 95 DEG C, obtains intermediate product 2, it is intermediate
Product 2 with 20g reacting ethylenediamine, reacts 3.0h at 60 DEG C, obtains drilling fluid polyamine shale inhibitor again.Yield is
96.48%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 7 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 6 is prepared has Formulas I structure, and in Formulas I, m takes 2, n to take 4, o
Take 2.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 7 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 8
10g epoxychloropropane is reacted under 60g catalyzed by amino sulfonic acid, 2.0h is reacted at 105 DEG C, obtains chloro two
Alcohol；The pure and mild 20g pentaethylene hexamine of above-mentioned chloro two is reacted, 3.0h is reacted at 60 DEG C, obtains intermediate product 1；It will be intermediate
Product 1,15g ethanol amine are reacted with 1.2g thionyl chloride, react 2.0h at 95 DEG C, obtain intermediate product 2, intermediate product 2
Again with 20g reacting ethylenediamine, 3.0h is reacted at 60 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 96.55%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 8 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 8 is prepared has Formulas I structure, and in Formulas I, m takes 1, n to take 4, o
Take 1.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 8 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Embodiment 9
10g epoxychloropropane is reacted under 60g catalysis of phosphotungstic acid, 2.0h is reacted at 105 DEG C, obtains chloro two
Alcohol；The pure and mild 20g pentaethylene hexamine of above-mentioned chloro two is reacted, 3.0h is reacted at 60 DEG C, obtains intermediate product 1；It will be intermediate
Product 1,15g ethanol amine are reacted with 1.2g thionyl chloride, react 2.0h at 95 DEG C, obtain intermediate product 2, intermediate product 2
Again with 20g reacting ethylenediamine, 3.0h is reacted at 60 DEG C, obtains drilling fluid polyamine shale inhibitor.Yield is 96.58%.
Infrared spectroscopy detection is carried out with polyamine shale inhibitor to the drilling fluid that the embodiment of the present invention 9 is prepared, is examined
Surveying result is that the polyamine shale inhibitor that the embodiment of the present invention 9 is prepared has Formulas I structure, and in Formulas I, m takes 1, n to take 4, o
Take 1.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that the embodiment of the present invention 9 is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
Comparative example 1
Drilling fluid polyamine shale inhibitor is prepared according to method described in embodiment 9, as different from Example 9,
Do not add thionyl chloride.
According to method described in above-mentioned technical proposal, the drilling fluid polyamine mud that comparative example 1 of the present invention is prepared is tested
The performance of shale control agent；Test result is as shown in table 1.
The drilling fluid polyamine shale inhibitor that 1 embodiment of the present invention of table and comparative example are prepared
It can test result
As shown in Table 1, drilling fluid polyamine shale inhibitor water prepared by the embodiment of the present invention that mass concentration is 1%
Solution rolls 16h, shale primary recovery > 96%, shale relative recovery > 99% in 150 DEG C of high temperature, and clay is opposite to be inhibited
Rate > 97%, extreme boundary lubrication coefficient < 0.08, EC50Value > 480000mg/L, drilling fluid polyamine shale inhibitor and routine
Water-base drilling fluid can be compounded with arbitrary proportion does not influence rheological property.The drilling fluid that the embodiment of the present invention is prepared polyamine mud
Shale control agent has preferable shale inhibition energy, clay stability, lubricity and compatibility, and inanimate object poison
Property.
As seen from the above embodiment, the present invention provides a kind of drilling fluid preparation method of polyamine shale inhibitor,
Include: to react chloro epoxides, acidic catalyst, polyethylene polyamine, ethanol amine, thionyl chloride and ethylenediamine, obtains
To drilling fluid polyamine shale inhibitor.The present invention prepares polyamine shale inhibitor using specific raw material, especially exists
Thionyl chloride is added in prepared composition, inhibits the drilling fluid being prepared with preferable shale with polyamine shale inhibitor
Property and clay stability.Moreover, the polyamine shale inhibitor that method provided by the invention is prepared also has preferably
Greasy property and compatibility, and no biotoxicity.Polyamine shale inhibitor provided by the invention can be applied to drilling fluid
In, suitable for requiring higher strong retraction mud shale, containing caving grounds and shale gas Horizontal Well Drilling well constructions such as mud stone.
What has been described above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill of the art
For personnel, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of drilling fluid preparation method of polyamine shale inhibitor, comprising:
Chloro epoxides, acidic catalyst, polyethylene polyamine, ethanol amine, thionyl chloride and ethylenediamine are reacted, obtained
Drilling fluid polyamine shale inhibitor.
2. the method according to claim 1, wherein the preparation method of drilling fluid polyamine shale inhibitor has
Body the following steps are included:
(1) chloro epoxides is reacted under acidic catalyst catalysis, obtains chloro glycol；
(2) the pure and mild polyethylene polyamine of chloro two is reacted, obtains the first intermediate product；
(3) the first intermediate product, ethanol amine and thionyl chloride are reacted, obtains the second intermediate product；
(4) the second intermediate product and ethylenediamine are reacted, obtains drilling fluid polyamine shale inhibitor.
3. the method according to claim 1, wherein chloro epoxides includes epoxychloropropane or 1,2- epoxy
Chloro-butane.
4. the method according to claim 1, wherein polyethylene polyamine include diethylenetriamine, triethylene tetramine,
Tetraethylenepentamine or pentaethylene hexamine.
5. the method according to claim 1, wherein the acidic catalyst includes hydrochloric acid, sulfuric acid, phosphoric acid, wine
Stone acid, oxalic acid, p-methyl benzenesulfonic acid, dodecyl benzene sulfonic acid, sulfamic acid or phosphotungstic acid.
6. according to the method described in claim 2, it is characterized in that, the temperature reacted in step (1) is 85~105 DEG C；
The time of reaction is 0.5~2 hour.
7. according to the method described in claim 2, it is characterized in that, the temperature reacted in step (2) is 45~60 DEG C；
The time of reaction is 1.5~3.0 hours.
8. according to the method described in claim 2, it is characterized in that, the temperature reacted in step (3) is 80~95 DEG C；Reaction
Time is 0.5~2.0 hour；
The temperature reacted in step (4) is 45~60 DEG C；The time of reaction is 1.5~3.0 hours.
9. a kind of drilling fluid polyamine shale inhibitor has structure shown in Formulas I:
In Formulas I, it be 1~4, o is 1~2 that m, which is 1~2, n,.
10. a kind of drilling fluid, the drilling fluid polyamine shale inhibitor being prepared including method described in claim 1；
Or drilling fluid as claimed in claim 9 polyamine shale inhibitor.
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| Publication number | Priority date | Publication date | Assignee | Title |
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