CN104592955B - A kind of polyamine shale control agent and preparation method thereof - Google Patents
A kind of polyamine shale control agent and preparation method thereof Download PDFInfo
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- CN104592955B CN104592955B CN201310530808.6A CN201310530808A CN104592955B CN 104592955 B CN104592955 B CN 104592955B CN 201310530808 A CN201310530808 A CN 201310530808A CN 104592955 B CN104592955 B CN 104592955B
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
- C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
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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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Abstract
The present invention discloses a kind of preparation method of polyamine class shale control agent, including following content：（1）Cyclic ethers is added into polyethylene polyamine under the conditions of stirring and 50~90 DEG C, polyethylene polyamine is 1 with the cyclic ethers mol ratio added：2~3, the reaction time is 1~4h；（2）By step（1）Temperature of charge rises to and epoxychloropropane is added under 70~110 DEG C, stirring condition, and the mol ratio of epoxychloropropane and polyethylene polyamine is 0.4~0.9:1, the reaction time is 1~3h；（3）To step（2）Material in add terminator, the mol ratio of terminator and polyethylene polyamine is 1~2.5:1, the reaction time is 1~2h, and polyamine class shale control agent is made after reaction.The polyamine class shale control agent of the present invention is while with superior mud shale rejection, hence it is evident that improve compatibility, and synthetic method is simple, and cost is low, without special odor, environment-friendly.
Description
Technical field
The present invention relates to a kind of polyamine shale control agent and preparation method thereof.
Background technology
Drilling fluid refers to during oil/gas drilling, met with its a variety of function drilling well demand various circulation of fluids it is total
Claim.The function of drilling fluid mainly has：Carry and suspension drilling cuttings；Stabilizing borehole and equilibrium strata pressure；Cooling and lubrication drill bit, brill
Tool；Transmit hydrodynamic force.
With the development of petroleum exploration domain, deep-well, ultradeep well, the appearance of ocean well and complex ground well, drilling well difficulty
Increase, the requirement to drilling fluid system is also more and more strict.Particularly during oil gas drilling, when boring chance mud shale stratum, mud
The hydration swelling of shale, scattered it will cause a series of problems, such as borehole well instability, bit balling and hole cleaning.Traditional oil base is bored
Well liquid, possesses many good performances, but it pollutes environment, using being restricted.Using polyamine class as the height of main shale control agent
Performance water-base drilling fluid turns into the research that countries in the world oil researcher pays close attention to its characteristic such as environmentally friendly, inexpensive, functional
Focus.
Poly- amine polymer is as main shale inhibitor, its mechanism of action：Adsorbed by the way that amido is distinctive
Effect, low molecule amine penetrates clay layer as potassium ion, exchangeable cations of the amine desorption with hydration shell of low concentration,
Clay lamella is bound together by Electrostatic Absorption, hydrogen bond action and dipole effect etc., prevents hydrone from entering, plays shale
The effect of suppression.
Polyamine class shale control agent is main based on macrocation, small cation.Macrocation is polyamine methacryl
Amine quaternary ammonium salt, inhibitor is coated with as clay；Small cation is epoxypropyltrimethylchloride chloride.Small cation molecular weight
It is small, with positive charge, surface of clay is easily adsorbed in, and enter between argillic horizon, substitution exchangeable cations is adsorbed in wherein.And its
Surface at binding molecule is the hydrophobic surface containing hydrocarbon group, is conducive to preventing hydrone from entering, therefore can effectively press down
The hydration swelling of clay processed and scattered.
Polyether amine inhibitor is the ULTRADRIL that MISWACO companies of the U.S. release in recent yearsTMHighly inhibited water-based drilling
Liquid.It is Patel et al. develop do not hydrolyze, water-soluble, low toxicity and match somebody with somebody completely with other conventional water-based drilling solution additives
5, its shale inhibition can be better than size cationic polymer.
Chinese patent CN 1069755A describe all kinds of performances of drilling fluid using big small cation as shale control agent, greatly
Small cation drilling fluid system shale inhibition can be preferably.The B2 of United States Patent (USP) US 7012043 describe polyether amine inhibitor,
Such inhibitor shows good mud shale rejection ability.Connected between macrocation backbone structure or side chain and main chain with C-C keys,
Branched fraction contains C-N keys；Small cation contains C-C, C-N ,-O- keys.Polyether amine inhibitor based on C-C ,-O-, in chain or
The end of the chain contains a small amount of C-N keys.The basic reason of the strong rejection capability of polyether amine be in its main chain or the end of the chain a small amount of multiple amine
The result that base is acted on simultaneously, therefore the ability of its constraint hydration and expansion of clay is stronger, shows strong rejection capability.
CN201110313847.1 describes a kind of preparation method of cationic polyamine shale control agent, to hold diamines, cyclic ethers, epoxy chlorine
Propane is raw material, aggregated rear obtained.Although the shale control agent inhibition is protruded, its compatibility with drilling fluid system
Need further raising.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of polyamine class shale control agent and preparation method thereof.The present invention
Polyamine class shale control agent while with superior mud shale rejection, hence it is evident that improve compatibility, and synthesis side
Method is simple, and cost is low, without special odor, environment-friendly.
A kind of preparation method of polyamine class shale control agent, including following content：
（1）Cyclic ethers, polyethylene polyamine and the ring added are added into polyethylene polyamine under the conditions of stirring and 50~90 DEG C
Ether mol ratio is 1：2~3, the reaction time is 1~4h；Preferable reaction temperature is 65~75 DEG C, polyethylene polyamine and the ring added
Ether mol ratio is 1：2~2.5, the reaction time is 2~3h；
（2）By step（1）Temperature of charge rises to 70~110 DEG C, and preferably 85~100 DEG C, epoxy chlorine is added under stirring condition
The mol ratio of propane, epoxychloropropane and polyethylene polyamine is 0.4~0.9:1, preferably 0.5~0.8:1, the reaction time be 1~
3h, preferably 1.5~2h；
（3）To step（2）Material in add terminator, the mol ratio of terminator and polyethylene polyamine is 1~2.5:1,
It is preferred that 1~1.8:1, the reaction time is 1~2h, preferably 1~1.5h, and polyamine class shale control agent is made after reaction.
Polyethylene polyamine described in the inventive method is diethylenetriamine, triethylene tetramine, TEPA, five ethene
Hexamine etc..Described cyclic ethers is oxirane, expoxy propane etc..Described terminator can be hydrochloric acid, sulfuric acid, nitric acid, ice vinegar
Acid, citric acid, formic acid, acetic acid；Can also be water, preferably the latter.When using water as terminator, by some in polymer
The hydrolysis of group carrys out the progress of terminating reaction, can further improve the compatibility of inhibitor.
A kind of polyamine class shale control agent, is prepared using the above method, with following structural formula：
Wherein, when n is 1~6 integer, n=1, raw material is diethylenetriamine, by that analogy；M is 0~1 integer, m=0
When, raw material is oxirane, and raw material is expoxy propane during m=1；K is the integer less than 15.
Compared with prior art, polyamine shale control agent of the invention has the following advantages that：
（1）The inventive method is using polyethylene polyamine as main Material synthesis, and obtained polyamine shale control agent is having excellent
Rejection while, compatibility is greatly enhanced, and can be used in a variety of drilling fluid systems；
（2）Result of study shows there is the polyethylene polyamine and end diamines of same atoms number, polyethylene polyamine on main chain
Reactivity will apparently higher than end diamines, this cause the present invention can be carried out under relatively low reaction temperature, with prior art
Compare, at the same reaction temperature, the reaction time substantially shortens, effectively reduction operational danger and synthesis cost.
Embodiment
The effect and effect of the inventive method are illustrated with reference to embodiment, but following examples are not constituted to this
The limitation of scheme of the invention.
Embodiment 1
Reaction temperature is set as 65 DEG C first, stirs and oxirane is passed through in diethylenetriamine, diethylenetriamine
Mol ratio with oxirane is 1：2, controlling reaction temperature is not less than 60 DEG C, reacts 3h；Then temperature is risen into 80 DEG C, stirring
Under the conditions of be added dropwise epoxychloropropane, the mol ratio of epoxychloropropane and diethylenetriamine is 0.6:1, the reaction time is 2h, finally
The mol ratio of addition terminator concentrated hydrochloric acid, concentrated hydrochloric acid and diethylenetriamine is 1:Polyamine class shale is made after 1, reaction 1h to suppress
Agent.
Embodiment 2
Reaction temperature is set as 75 DEG C, stirs and simultaneously expoxy propane is added drop-wise in triethylene tetramine, triethylene tetramine with
The mol ratio of expoxy propane is 1：3, controlling reaction temperature is not less than 70 DEG C, reacts 2h；Then temperature is risen into 90 DEG C, stirring bar
It is added dropwise epoxychloropropane under part, the mol ratio rubbed of epoxychloropropane and diethylenetriamine is 0.5:1, the reaction time is 3h；Most
Terminator formic acid is added afterwards, and the mol ratio of formic acid and diethylenetriamine is 1.5:Polyamine class shale is made after 1, reaction 1.5h to suppress
Agent.
Embodiment 3
Reaction temperature is set as 85 DEG C, stirs and simultaneously expoxy propane is added drop-wise in TEPA, TEPA with
The mol ratio of expoxy propane is 1：2.5, controlling reaction temperature is not less than 80 DEG C, reacts 1.5h；Then temperature is risen to 100 DEG C,
It is added dropwise epoxychloropropane under stirring condition, the mol ratio rubbed of epoxychloropropane and diethylenetriamine is 0.8:1, the reaction time is
2h；It is eventually adding terminator acetic acid, the mol ratio of acetic acid and diethylenetriamine is 1.8:Polyamine class shale is made after 1, reaction 1h
Inhibitor.
Embodiment 4
Preparation process be the same as Example 1, simply terminator be adjusted to water.
Embodiment 5
Preparation process be the same as Example 2, simply terminator be adjusted to water.
Embodiment 6
Preparation process be the same as Example 3, simply terminator be adjusted to water.
Comparative example 1
Reaction temperature is set as 75 DEG C first, stirs and oxirane is passed through in hexamethylene diamine, hexamethylene diamine and epoxy second
The mol ratio of alkane is 1：2, controlling reaction temperature is not less than 70 DEG C, reacts 3h；Then temperature is risen to 90 DEG C, dripped under stirring condition
Plus epoxychloropropane, the mol ratio of epoxychloropropane and hexamethylene diamine is 0.6:1, the reaction time is 2h, is eventually adding terminator dense
The mol ratio of hydrochloric acid, concentrated hydrochloric acid and hexamethylene diamine is 1:Polyamine class shale control agent is made after 1, reaction 1h.
The evaluation method of polyamine inhibitor prepared by above-described embodiment and comparative example is as follows：
（1）Relative inhibition
350 milliliters of distilled water are taken, 1.05g is added（It is accurate to 0.01g）Sodium carbonate, 5min is stirred under 10000r/min
Afterwards, it is slowly added to 35g（It is accurate to 0.01g）Drilling fluid bentonite, 20min is stirred under 10000r/min, the heat at 120 DEG C
16h is rolled, 5min is stirred under 10000 ± 300r/min after cooling, the value of base slurry is determined at 24 ± 3 DEG C.
Take the sample of certain mass to be dissolved in 350 milliliters of distilled water, stir, add 1.05g（It is accurate to 0.01g）
Sodium carbonate, stirs after 5min under 10000r/min, is slowly added to 35g（It is accurate to 0.01g）Drilling fluid bentonite,
20min is stirred under 10000r/min, heat rolling 16h, stirs 5min, 24 after cooling under 10000 ± 300r/min at 120 DEG C
Location survey determines the value of mud at ± 3 DEG C.
（2）Compatibility is evaluated
The inhibitor of each concentration is added in different drilling fluid systems, 20min is stirred with 8000r/min rotating speeds, at 70 DEG C
Room temperature is down in lower aging 16h, taking-up, and 5min is stirred with 8000r/min rotating speeds, measures property of drilling fluid situation of change.
Different polyamine contrast test results are as follows：Following % is weight/mass percentage composition.
The relative inhibition of the different polyamine inhibitors of table 1
Experiment condition：120 DEG C of heat rolling 16h, bentonite mass concentration 10%
The compatibility of table 2 and polymer drilling fluid
Polymer drilling fluid is formulated：4%~6%+PAC of bentonite (fluid loss additive) 0.1%+JT-888 (fluid loss additive) 0.2%
~0.3%+FA-367 (coating agent) 0.4%~0.6%+RH-3 (lubricant) 0.4%~0.6%
AV is that apparent viscosity, PV are that plastic viscosity, YP are that yield value, Gel are gel strength（Front and rear numerical value is respectively to ingress
And egress）, FL be filter loss.Each index is compared with base slurry data, and less fluctuation difference is preferred, and illustrates that compatibility is good
It is good.
The compatibility of table 3 and sulphonated polymer mud
Sulphonated polymer mud is formulated：4%~6%+ of bentonite PAC (fluid loss additive) 0.1%+SMP-1 (fluid loss additive) 2.0%+
SMT (thinner) 0.2%~0.5%+QS-2 (plugging material) 2.0%+ RH-3 (lubricant) 0.4%~0.6%.
Claims (7)
1. a kind of preparation method of polyamine class shale control agent, it is characterised in that：Including following content：
（1）Cyclic ethers is added into polyethylene polyamine under the conditions of stirring and 50~90 DEG C, polyethylene polyamine rubs with the cyclic ethers added
You are than being 1：2~3, the reaction time is 1~4h；
（2）By step（1）Temperature of charge rises to and epoxychloropropane is added under 70~110 DEG C, stirring condition, epoxychloropropane with it is many
The mol ratio of ethylene polyamine is 0.4~0.9:1, the reaction time is 1~3h；
（3）To step（2）Material in add terminator, the mol ratio of terminator and polyethylene polyamine is 1~2.5:1, reaction
Time is 1~2h, and polyamine class shale control agent is made after reaction, wherein, described terminator is water.
2. according to the method described in claim 1, it is characterised in that：Step（1）Middle reaction temperature is 65~75 DEG C, and many ethene are more
Amine is 1 with the cyclic ethers mol ratio added：2~2.5, the reaction time is 2~3h.
3. according to the method described in claim 1, it is characterised in that：Step（1）Described in polyethylene polyamine be divinyl three
One or more in amine, triethylene tetramine, TEPA, pentaethylene hexamine.
4. according to the method described in claim 1, it is characterised in that：Step（1）Described in cyclic ethers be oxirane, epoxy third
Alkane.
5. according to the method described in claim 1, it is characterised in that：Step（2）Middle temperature of charge rises to 85~100 DEG C, epoxy
The mol ratio of chloropropane and polyethylene polyamine is 0.5~0.8:1, the reaction time is 1.5~2h.
6. according to the method described in claim 1, it is characterised in that：Step（3）The mol ratio of middle terminator and polyethylene polyamine
For 1~1.8:1, the reaction time is 1~1.5h.
7. the polyamine class shale control agent prepared by a kind of use claim 1 to 6 either method, with following structural formula：
Wherein, when n is 1~6 integer, n=1, raw material is diethylenetriamine, by that analogy；It is former when m is 0~1 integer, m=0
Expect for oxirane, raw material is expoxy propane during m=1；K is the integer less than 15.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038738A (en) * | 2015-07-14 | 2015-11-11 | 中国石油天然气集团公司 | High-temperature resistant efficient mud shale inhibitor for drilling fluid and preparation method therefor |
| CN105086955B (en) * | 2015-08-27 | 2018-03-13 | 中国石油集团渤海钻探工程有限公司 | Polyamine inhibitor for water-based drilling fluid and preparation method thereof |
| CN105647506B (en) * | 2016-01-21 | 2018-12-21 | 中国石油化工股份有限公司 | Oil-gas field fracturing clay stabilizer and preparation method thereof |
| CN106350036B (en) * | 2016-08-22 | 2018-11-06 | 西南石油大学 | A kind of synthetic method of alkyl tetramine, four amine product of alkyl and its shale control agent |
| CN109439292A (en) * | 2018-10-22 | 2019-03-08 | 新疆水处理工程技术研究中心有限公司 | Clay stabilizer |
| CN112175592B (en) * | 2019-07-02 | 2022-11-29 | 中石化南京化工研究院有限公司 | Dendritic cationic polyacrylamide coating agent for water-based drilling fluid and preparation method thereof |
| CN111718698B (en) * | 2020-07-22 | 2022-04-19 | 西南石油大学 | Hyperbranched polyetheramine environment-friendly shale inhibitor, preparation method thereof and water-based drilling fluid |
| CN115403786B (en) * | 2021-05-28 | 2023-09-19 | 中石化石油工程技术服务有限公司 | Humic acid shale inhibitor and preparation method and application thereof |
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