CN107652954A - A kind of nitrogen heterocyclic ring solid crosslinking agent and its preparation method and application - Google Patents
A kind of nitrogen heterocyclic ring solid crosslinking agent and its preparation method and application Download PDFInfo
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- CN107652954A CN107652954A CN201710884340.9A CN201710884340A CN107652954A CN 107652954 A CN107652954 A CN 107652954A CN 201710884340 A CN201710884340 A CN 201710884340A CN 107652954 A CN107652954 A CN 107652954A
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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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of nitrogen heterocyclic ring solid crosslinking agent and its preparation method and application, belong to technical field of oilfield chemistry.According to mass percent, the crosslinking agent is made up of 40% 45% triamine of 1,3,5 triazine 2,4,6,40% 45% hexa and 10% 20% stabilizer.The crosslinking agent in preparing cross-linked polymer gel profile control agent when applying, 70 DEG C of gelling temperature 40 DEG C, and gelation time 2 days to 7 days is controllable, and final set viscosity is up to more than 8000mPas, and the gel rubber system of formation is stable, and gel strength retention is more than 80% within 90 days.Intake profile can be effectively adjusted, realizes the efficient closure in target zone, improves oil recovery factor.
Description
Technical field
The present invention relates to technical field of oilfield chemistry, more particularly to a kind of nitrogen heterocyclic ring solid crosslinking agent and preparation method thereof
And application.
Background technology
Well water is especially tail period common problem in oilfield development process, and injection water is often along hypertonic
Permeable layers penetrate into oil well, have a strong impact on water flooding effectiveness, reduce oil field harvest efficiency, cause oil well productivity to decline.For in solution
Problem is stated, the water plugging and profiling technology of oil reservoir is paid attention to and developed in the exploitation of oil gas field.Crosslinking agent is Water in Water Shutoff in Oil Field profile control
During commonly use chemical reagent, can react to obtain the gel of different viscosities with polyacrylamide polymer, realize to infiltration
The selective shut-off of layer.
The gelation time of currently used metallic-ion crosslinking agent is short, and heat endurance is poor, during its application is confined to
Low-temperature reservoir.The bio-toxicity of organic phenolic crosslinkers is larger, the easy spontaneous polymerization when liquid is matched somebody with somebody on ground, construction success rate compared with
It is low.Therefore oil field development field need develop gelation time it is more controllable, heat endurance is more preferable, more environmentally friendly crosslinking agent and its water blockoff
Profile control system.
The content of the invention
It is an object of the invention to provide a kind of nitrogen heterocyclic ring solid crosslinking agent, the crosslinking agent safety and environmental protection and heat endurance
Good, gelation time and gelling strength are adjustable.
The present invention also aims to provide the preparation method and application of above-mentioned nitrogen heterocyclic ring solid crosslinking agent.
On the one hand, to achieve the above object, the invention provides a kind of nitrogen heterocyclic ring solid crosslinking agent, according to quality percentage
1,3,5-triazines -2,4 than, the crosslinking agent by 40%-45%, 6- triamines, 40%-45% hexa and
10%-20% stabilizer composition.
Further, the stabilizer is one or both of thiocarbamide and sodium sulfite.
Further, the stabilizer is made up of the thiocarbamide and sodium sulfite that mass ratio is 2~3: 1.
Further, the stabilizer is made up of the thiocarbamide and sodium sulfite that mass ratio is 2: 1.
On the other hand, the invention provides a kind of preparation method of nitrogen heterocyclic ring solid crosslinking agent, including：By quality percentage
Than 1,3,5- triazine -2,4,6- triamines, 40%-45% hexa and the 10%-20% stabilization for 40%-45%
Agent is sufficiently mixed, and is stirred as the nitrogen heterocyclic ring solid crosslinking agent.
On the other hand, the invention provides a kind of nitrogen heterocyclic ring solid crosslinking agent to prepare cross-linked polymer gel profile control agent
In application.
Further, the method for the application includes：
The polyacrylamide solution that mass fraction is 0.2%-0.4% is prepared, liquid must be cured after curing；
The nitrogen heterocyclic ring solid crosslinking agent is added into the curing liquid, and adjusts the pH value of solution in the range of 5-6,
Stir to obtain base fluid；Wherein, the addition of the nitrogen heterocyclic ring solid crosslinking agent is the polyacrylamide solution quality
0.2%-0.4%；
The base fluid is reacted at a temperature of 40 DEG C -70 DEG C and obtains the gel with three-dimensional net structure, the gel
As described cross-linked polymer gel profile control agent.
Further, the relative molecular mass of the polyacrylamide is 20,000,000-2,500 ten thousand, degree of hydrolysis 15%-
20%.
One or more of the embodiment of the present application technical scheme, has at least the following technical effects or advantages：
The nitrogen heterocyclic ring solid crosslinking agent that the embodiment of the present application provides, the crosslinking agent safety and environmental protection, at 40 DEG C -70 DEG C
Plastic, heat endurance is good, and gelation time and gelling strength are adjustable, available for the deep profile controlling of oil reservoir, improves oil recovery.
Brief description of the drawings
Fig. 1 is nitrogen heterocyclic ring solid crosslinking agent answering in cross-linked polymer gel profile control agent is prepared in the embodiment of the present application
Use method flow diagram.
Embodiment
The embodiment of the present application provides a kind of nitrogen heterocyclic ring solid crosslinking agent and its preparation method and application, crosslinking agent safety
Environmental protection, 40 DEG C -70 DEG C can plastic, heat endurance is good, and gelation time and gelling strength are adjustable, available for oil reservoir deep adjust
Cut open, improve oil recovery.
To achieve the above object, the embodiment of the present application general thought is as follows：
This application provides a kind of nitrogen heterocyclic ring solid crosslinking agent, and according to mass percent, the crosslinking agent is by 40%-
The stabilizer composition of 45% 1,3,5- triazine -2,4,6- triamines, 40%-45% hexa and 10%-20%.
The nitrogen heterocyclic ring solid crosslinking agent of the application, with 1,3,5-triazines -2,4,6- triamines, hexa and stably
Agent is raw material, in acid condition reaction play crosslinked action, 40 DEG C -70 DEG C can plastic, gelation time 2 days to 7 days, into
Glue time and gelling strength are adjustable, and without phenolic toxic compounds, safety and environmental protection, and heat endurance are good.
In order to be better understood from above-mentioned technical proposal, below by accompanying drawing and specific embodiment to technical scheme
It is described in detail, it should be understood that the specific features in the embodiment of the present application and embodiment are to the detailed of technical scheme
Thin explanation, rather than the restriction to technical scheme, in the case where not conflicting, the embodiment of the present application and embodiment
In technical characteristic can be combined with each other.
On the one hand, the embodiment of the present application provides a kind of nitrogen heterocyclic ring solid crosslinking agent, according to mass percent, the friendship
Join agent by the steady of 40%-45% 1,3,5- triazine -2,4,6- triamines, 40%-45% hexa and 10%-20%
Determine agent composition.
The implication of term " stabilizer " used in the embodiment of the present application is that can slow down crosslinking agent itself polycondensation reaction,
Extend a kind of chemical addition agent of the crosslinking agent term of validity.Stabilizer described in the embodiment of the present application is in thiocarbamide and sodium sulfite
It is one or two kinds of.
Wherein, when stabilizer selects two kinds of thiocarbamide and sodium sulfite, its mass ratio is 2~3: 1, preferably 2: 1.
The effect to each component in the embodiment of the present application and the mechanism of action elaborate below：
1,3,5-triazines -2,4, skeleton structure of the 6- triamines as crosslinking agent, in acid condition hexa energy
Enough and 1,3,5-triazines -2,4,6- triamines obtain polyhydroxy methyl structural molecule, and the molecule can play crosslinked action.The two is used
Otherwise amount can need to cause to react insufficient in OK range, or cause excessively to be crosslinked, and can cross-linking properties is deteriorated.Surely
Determine agent and play oxygen in removing system, be complexed the effect of high volence metal ion, reduce plastic system rates of oxidative degradation, improve anti-
Metal ion ability；The too small stablizing effect unobvious of its dosage, dosage, which crosses conference, causes gelling strength to reduce.
The crosslinking agent of the application is free of phenolic toxic compounds, safety and environmental protection；Not metal ion, gelation time and into
Glue intensity is adjustable, and heat endurance is good.In addition, solid crosslinking agent compared with liquid cross-linker, can effectively avoid phenolic aldehyde class I liquid I from handing over
Molecule slow reaction causes the problem of solidification failure in the short time in connection agent, has the technique effect of long shelf-life, and convenient storage
Deposit, transport and use.
On the other hand, based on same inventive concept, the embodiment of the present application provides a kind of above-mentioned nitrogen heterocyclic ring solid crosslinking
The preparation method of agent, it is specially：
It is 40%-45% 1,3,5- triazine -2,4,6- triamines by mass percent, 40%-45% hexa-methylene four
Amine and 10%-20% stabilizer are sufficiently mixed, and are stirred as the nitrogen heterocyclic ring solid crosslinking agent.
On the other hand, based on same inventive concept, the embodiment of the present application provides a kind of described nitrogen heterocyclic ring solid and handed over
Join application of the agent in cross-linked polymer gel profile control agent is prepared.
Fig. 1 is refer to, the application process specifically includes following steps：
Step S110：The polyacrylamide solution that mass fraction is 0.2%-0.4% is prepared, liquid must be cured after curing；
Term " curing " used in the embodiment of the present invention is to instigate polyacrylamide fully to be dissolved in water, and strand is in fully exhibition
Open state.
Step S120：Add the nitrogen heterocyclic ring solid crosslinking agent into the curing liquid, and adjust the pH value of solution to
In the range of 5-6, stir to obtain base fluid；Wherein, the addition of the nitrogen heterocyclic ring solid crosslinking agent is the polyacrylamide
The 0.2%-0.4% of aqueous solution quality；
PH value selection 5-6 be because catabolite of the hexa in this pH value range and 1,3,5- triazine -2,
The reactivity highest of 4,6- triamines, be advantageous to improve the crosslinking active of crosslinking agent.Specifically, acetic acid, hydrochloric acid and lemon can be used
Any one or a few regulation system pH value in lemon acid is in the range of 5-6.
Step S130：The base fluid is reacted at a temperature of 40 DEG C -70 DEG C and obtains the gel with three-dimensional net structure,
The gel is the cross-linked polymer gel profile control agent.
Wherein, the polyacrylamide is anion-polyacrylamide, and relative molecular mass is 20,000,000-2,500 ten thousand,
Degree of hydrolysis is 15%-20%.
The profile control agent prepared by the above method, 40 DEG C -70 DEG C of gelling temperature, gelation time controllable, final set in 2 days to 7 days
Viscosity is up to more than 8000mPas, and the gel rubber system of formation is stable, and gel strength retention is more than 80% within 90 days.Can effectively it adjust
Whole intake profile, the efficient closure in target zone is realized, improve oil recovery factor.
In order that those skilled in the art can further understand the scheme of the embodiment of the present application, will be based on below
The scheme that the embodiment of the present application is introduced describes in detail to it.
Embodiment 1
1,3,5-triazines -2,4 is weighed respectively, and 6- triamine 40g, hexa 40g, anhydrous sodium sulfite 20g will be upper
State raw material to be sufficiently mixed, stir as nitrogen heterocyclic ring solid crosslinking agent.
The application of the nitrogen heterocyclic ring solid crosslinking agent, specifically includes following steps：
Partially hydrolyzed polyacrylamide (PHPA) is added to the water under rapid stirring obtain mass concentration be 0.2% it is poly-
Acrylamide solution, curing must cure liquid in 24 hours；Then 0.2% nitrogen heterocyclic ring solid crosslinking agent is added, is adjusted using acetic acid
Section system pH to 5-6, base fluid must be reacted after stirring；The reaction base fluid is placed in into constant temperature to plastic in 60 DEG C of baking oven to obtain
To profile control agent.Gelation time is 5 days, is 11250mPas into adhesiveness.
Embodiment 2
1,3,5-triazines -2,4,6- triamine 44g, hexa 44g, thiocarbamide 8g, anhydrous sodium sulfite are weighed respectively
4g, above-mentioned raw materials are sufficiently mixed, stirred as nitrogen heterocyclic ring solid crosslinking agent.
The application of the nitrogen heterocyclic ring solid crosslinking agent, specifically includes following steps：
Partially hydrolyzed polyacrylamide (PHPA) is added to the water under rapid stirring obtain mass concentration be 0.3% it is poly-
Acrylamide solution, curing must cure liquid in 24 hours；Then 0.3% nitrogen heterocyclic ring solid crosslinking agent is added, is adjusted using acetic acid
Section system pH to 5-6, base fluid must be reacted after stirring；The reaction base fluid is placed in into constant temperature to plastic in 60 DEG C of baking oven to obtain
To profile control agent.Gelation time is 3 days, is 11110mPas into adhesiveness.
Embodiment 3
1,3,5-triazines -2,4 is weighed respectively, and 6- triamine 42g, hexa 42g, anhydrous sodium sulfite 16g will be upper
State raw material to be sufficiently mixed, stir as nitrogen heterocyclic ring solid crosslinking agent.
The application of the nitrogen heterocyclic ring solid crosslinking agent, specifically includes following steps：
Partially hydrolyzed polyacrylamide (PHPA) is added to the water under rapid stirring obtain mass concentration be 0.4% it is poly-
Acrylamide solution, curing must cure liquid in 24 hours；Then 0.4% nitrogen heterocyclic ring solid crosslinking agent is added, is adjusted using hydrochloric acid
Section system pH to 5-6, base fluid must be reacted after stirring；The reaction base fluid is placed in into constant temperature to plastic in 70 DEG C of baking oven to obtain
To profile control agent.Gelation time is 2 days, is 13123mPas into adhesiveness.
Embodiment 4
1,3,5-triazines -2,4 is weighed respectively, and 6- triamine 45g, hexa 45g, anhydrous sodium sulfite 10g will be upper
State raw material to be sufficiently mixed, stir as nitrogen heterocyclic ring solid crosslinking agent.
The application of the nitrogen heterocyclic ring solid crosslinking agent, specifically includes following steps：
Partially hydrolyzed polyacrylamide (PHPA) is added to the water under rapid stirring obtain mass concentration be 0.3% it is poly-
Acrylamide solution, curing must cure liquid in 24 hours；Then 0.3% nitrogen heterocyclic ring solid crosslinking agent is added, uses citric acid
Regulation system pH to 5-6, base fluid must be reacted after stirring；The reaction base fluid is placed in 40 DEG C of baking oven constant temperature to plastic
Obtain profile control agent.Gelation time is 6 days, is 12892mPas into adhesiveness.
Embodiment 5
1,3,5-triazines -2,4 is weighed respectively, 6- triamine 40g, hexa 40g, thiocarbamide 20g, above-mentioned raw materials is filled
Divide mixing, stir as nitrogen heterocyclic ring solid crosslinking agent.
The application of the nitrogen heterocyclic ring solid crosslinking agent, specifically includes following steps：
It is 0.35% that partially hydrolyzed polyacrylamide (PHPA) is added to the water under rapid stirring to obtain mass concentration
Polyacrylamide solution, curing must cure liquid in 24 hours；Then 0.35% nitrogen heterocyclic ring solid crosslinking agent is added, uses acetic acid
With citric acid regulation system pH to 5-6, base fluid must be reacted after stirring；The reaction base fluid is placed in 50 DEG C of baking oven permanent
Temperature to plastic obtains profile control agent.Gelation time is 5 days, is 12632mPas into adhesiveness.
Gel viscosity is tested using RS6000 rotational rheometers in the embodiment of the present application, from PZ38 rotors, test
Temperature is set as gelling temperature, rotating speed 1.5s-1, measure and average three times.Under different gelling temperatures test gel viscosity with
The change of time, gel thermal stability data is obtained, is shown in Table 1：
The gel heat endurance of table 1
As can be seen from Table 1,90 days gel strengths of cross-linked polymer gel profile control agent that prepared by the embodiment of the present application are possessed
For rate more than 80%, heat endurance is good, can effectively adjust intake profile, realizes the efficient closure in target zone, improves crude oil and adopts
Yield.
It should be noted last that above embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, it all should cover
Among scope of the presently claimed invention.
Claims (8)
1. a kind of nitrogen heterocyclic ring solid crosslinking agent, it is characterised in that according to mass percent, the crosslinking agent is by 40%-45%
1,3,5- triazine -2,4,6- triamines, 40%-45% hexa and 10%-20% stabilizer composition.
2. nitrogen heterocyclic ring solid crosslinking agent as claimed in claim 1, it is characterised in that the stabilizer is thiocarbamide and sulfurous acid
One or both of sodium.
3. nitrogen heterocyclic ring solid crosslinking agent as claimed in claim 2, it is characterised in that the stabilizer is 2~3 by mass ratio
: 1 thiocarbamide and sodium sulfite composition.
4. nitrogen heterocyclic ring solid crosslinking agent as claimed in claim 3, it is characterised in that the stabilizer is 2: 1 by mass ratio
Thiocarbamide and sodium sulfite composition.
5. the preparation method of the nitrogen heterocyclic ring solid crosslinking agent as described in one of claim 1-4, it is characterised in that including：Will
Mass percent is 40%-45% 1,3,5- triazine -2,4,6- triamines, 40%-45% hexa and 10%-
20% stabilizer is sufficiently mixed, and is stirred as the nitrogen heterocyclic ring solid crosslinking agent.
6. the nitrogen heterocyclic ring solid crosslinking agent as described in one of claim 1-4 is in cross-linked polymer gel profile control agent is prepared
Using.
7. application as claimed in claim 6, it is characterised in that the method for the application includes：
The polyacrylamide solution that mass fraction is 0.2%-0.4% is prepared, liquid must be cured after curing；
The nitrogen heterocyclic ring solid crosslinking agent is added into the curing liquid, and adjusts the pH value of solution in the range of 5-6, stirring
It is uniform to obtain base fluid；Wherein, the addition of the nitrogen heterocyclic ring solid crosslinking agent is the polyacrylamide solution quality
0.2%-0.4%；
The base fluid is reacted at a temperature of 40 DEG C -70 DEG C and obtains the gel with three-dimensional net structure, the gel is
The cross-linked polymer gel profile control agent.
8. application as claimed in claim 7, it is characterised in that the relative molecular mass of the polyacrylamide is 20,000,000-
25000000, degree of hydrolysis 15%-20%.
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| CN201710884340.9A CN107652954A (en) | 2017-09-26 | 2017-09-26 | A kind of nitrogen heterocyclic ring solid crosslinking agent and its preparation method and application |
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| CN201710884340.9A CN107652954A (en) | 2017-09-26 | 2017-09-26 | A kind of nitrogen heterocyclic ring solid crosslinking agent and its preparation method and application |
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Cited By (3)
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| CN110305638A (en) * | 2019-04-24 | 2019-10-08 | 中国石油化工股份有限公司 | A kind of sealing agent and its application |
| CN111363392A (en) * | 2020-04-08 | 2020-07-03 | Tcl华星光电技术有限公司 | Frame glue, display panel and preparation method thereof |
| CN112735704A (en) * | 2020-12-11 | 2021-04-30 | 河源市可顺绝缘材料有限公司 | Ultrahigh voltage-resistant insulating material and electric shock gun insulating wire using same |
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Application publication date: 20180202 |