CN106916578A - A kind of high temperature resistant Weak Gels type profile control agent and preparation method thereof - Google Patents
A kind of high temperature resistant Weak Gels type profile control agent and preparation method thereof Download PDFInfo
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- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
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- C09K8/506—Compositions based on water or polar solvents containing organic compounds
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- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
Abstract
The invention discloses a kind of high temperature resistant Weak Gels type profile control agent and preparation method thereof, belong to chemical water shutoff profile control agent field.The high temperature resistant Weak Gels type profile control agent includes：Partially hydrolyzed polyacrylamide (PHPA), concentration be the phenol-formaldehyde resin modified of 0.6g/L-2.0g/L, concentration be 0.5g/L-2.0g/L auxiliary agent and water of the concentration for 0.8g/L-2.5g/L.To phenol is added in reactor, 45-55 DEG C is heated to, base catalyst is added while stirring, be incubated 10-30min, formalin is instilled, is rapidly heated to 70-90 DEG C, be incubated 3-5h, urea is eventually adding, 10-30min is incubated after being well mixed, obtain phenol-formaldehyde resin modified.Phenol is 1 with the mol ratio of formaldehyde in formalin:2.7-3.3, amount of urea is the 1-5% of phenol and formalin gross mass.Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is added, reacted in the case where reaction system pH is 6-8 and stirring, auxiliary agent is obtained after sloughing moisture.The mol ratio of aluminium chloride, oxalic acid and ammonium chloride is 1:(15-30):(70-90).The high temperature resistant Weak Gels type profile control agent is resistant to 90-110 DEG C of high temperature, and the term of validity is long.
Description
Technical field
The present invention relates to chemical water shutoff profile control agent field, more particularly to a kind of high temperature resistant Weak Gels type profile control agent and
Its preparation method.
Background technology
At present, the most of oil fields of China are developed using water flooding regime to oil field, in development late stage, due to
The anisotropism on stratum, making the water of injection oil reservoir has 80%~90% to be absorbed by the little high-permeability reservoir of thickness,
Cause water injection profile very uneven, reduce the harvest efficiency of oil reservoir.In order to adjust the uniformity of water injection profile,
The sweep efficiency of injection water, the effect of low permeability formation in performance are improved, so that the recovery ratio of oil reservoir is improved,
It is accomplished by carrying out a certain degree of blocking to high-permeability reservoir, the chemical agent used during blocking referred to as profile control
Agent.And when profile control agent is Weak Gels system, it had both had certain intensity, high-permeability reservoir can be risen
To plugging action, and with certain mobility, can be slow to earth formation deep in high-permeability reservoir passage
It is mobile, with good profile control effect.Therefore it provides a kind of profile control agent with Weak Gels system very must
Will.
Prior art provides a kind of Weak Gels type profile control agent, is mixed by by the material of following mass fraction
Close：0.1~0.3 part of polyacrylamide, 0.05~0.2 part of methenamine, 0.005~0.03 part of resorcinol,
0.05~0.2 part of ammonium chloride, 0.01~0.05 part of sodium acid carbonate, 0.05~0.15 part of glacial acetic acid, 100 parts of water,
After mixing, the pH to 5 of solution is adjusted, toasted at 60-90 DEG C, obtain Weak Gels type profile control agent.
Inventor has found that prior art at least has following technical problem：
The profile control that the Weak Gels type profile control agent that prior art is provided is only capable of meeting when formation temperature is 60-90 DEG C will
Ask, when formation temperature is higher than 90 DEG C, the high temperature resistant property of the Weak Gels type profile control agent is poor and the term of validity is shorter,
The profile control of high-temperature stratum water filling cannot be met.
The content of the invention
The technical problems to be solved by the invention are, there is provided a kind of high temperature resistant and term of validity Weak Gels long
Type profile control agent and preparation method thereof, concrete technical scheme is as follows：
On the one hand, a kind of high temperature resistant Weak Gels type profile control agent is the embodiment of the invention provides, including：Part water
Solution polyacrylamide, phenol-formaldehyde resin modified, auxiliary agent and water；The partially hydrolyzed polyacrylamide (PHPA) concentration is 0.8
G/L-2.5g/L, the modified phenolic resin lipid concentration is 0.6g/L-2.0g/L, and the assistant concentration is 0.5
g/L-2.0g/L。
The phenol-formaldehyde resin modified is prepared via a method which to obtain：
To phenol is added in reactor, 45-55 DEG C is heated to, base catalyst is then added while stirring, protected
After warm 10-30min, then formalin is instilled, be rapidly heated to 70-90 DEG C, be incubated 3-5h, be eventually adding
Urea, 10-30min is incubated after being well mixed, and obtains the phenol-formaldehyde resin modified.The matter of the formalin
Amount concentration is 25-35%, and the phenol is 1 with the mol ratio of formaldehyde in the formalin:2.7-3.3, it is described
Amount of urea is the 1-5% of the phenol and the formalin gross mass.
The auxiliary agent is prepared via a method which to obtain：
Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is subsequently adding, is 6-8 in reaction system pH
And reacted under stirring, obtain the auxiliary agent after finally sloughing moisture.The aluminium chloride, oxalic acid
It is 1 with the mol ratio of ammonium chloride:(15-30):(70-90).
On the other hand, the embodiment of the present invention additionally provides a kind of side for preparing the high temperature resistant Weak Gels type profile control agent
Method, including：
Step a, prepare phenol-formaldehyde resin modified
To phenol is added in reactor, 45-55 DEG C is heated to, base catalyst is then added while stirring, protected
After warm 10-30min, then formalin is instilled, be rapidly heated to 70-90 DEG C, be incubated 3-5h, be eventually adding
Urea, 10-30min is incubated after being well mixed, and obtains the phenol-formaldehyde resin modified.The matter of the formalin
Amount concentration is 25-35%, and the phenol is 1 with the mol ratio of formaldehyde in the formalin:2.7-3.3, it is described
Urea is the 1-5% of the phenol and the formalin gross mass.
Step b, prepare auxiliary agent
Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is subsequently adding, is 6-8 in reaction system pH
And reacted under stirring, obtain the auxiliary agent after finally sloughing moisture.The aluminium chloride, oxalic acid
It is 1 with the mol ratio of ammonium chloride:(15-30):(70-90).
Step c, preparation high temperature resistant Weak Gels type profile control agent
The aqueous solution of partially hydrolyzed polyacrylamide (PHPA) is prepared, then to the water of the partially hydrolyzed polyacrylamide (PHPA)
The phenol-formaldehyde resin modified and the auxiliary agent are added in solution, is well mixed and is put into climatic chamber,
Constant temperature treatment is carried out at 90-110 DEG C, the high temperature resistant Weak Gels type profile control agent is obtained.The high temperature resistant Weak Gels
In type profile control agent, the concentration of the partially hydrolyzed polyacrylamide (PHPA) is 0.8g/L-2.5g/L, the modified phenolic
The concentration of resin is 0.6g/L-2.0g/L, and the concentration of the auxiliary agent is 0.5g/L-2.0g/L.
Specifically, preferably, the base catalyst is NaOH.
Specifically, preferably, the consumption of the base catalyst is that the formalin is total with the phenol
The 2-10% of quality.
Specifically, preferably, in the step a, the total time that instilling the formalin needs is
10-60min。
Specifically, preferably, in the step b, the pH that the reaction system is adjusted with ammoniacal liquor is 6-8.
Specifically, preferably, in the step c, the constant temperature process time is 8-40h.
Specifically, preferably, in the step c, the relative air humidity of the climatic chamber is 1-3%.
Specifically, preferably, in the step c, preparing the water-soluble of the partially hydrolyzed polyacrylamide (PHPA)
Liquid includes：The partially hydrolyzed polyacrylamide (PHPA) is added to the water, stirring curing 2-4h obtains the part
The aqueous solution of hydrolyzed polyacrylamide.
The beneficial effect that technical scheme provided in an embodiment of the present invention is brought is：
High temperature resistant Weak Gels type profile control agent provided in an embodiment of the present invention, using partially hydrolyzed polyacrylamide (PHPA) as
Host, by phenol-formaldehyde resin modified and host cross-linking reaction, and under the complex role of auxiliary agent, is formed
High temperature resistant Weak Gels type profile control agent is resistant to 90-110 DEG C of high temperature, and the term of validity is long.Wherein, by modified phenol
Urea is added in urea formaldehyde preparation process, it is reacted with free formaldehyde, so that in reducing phenolic resin
Free formaldehyde, the profile control agent for obtaining is more environmentally-friendly, meanwhile, urea also acts as the effect of stabilizer, suppresses weak
The decomposition of gel rubber system, makes Weak Gels system plastic after 30 days, in the high temperature bar that formation temperature is 90-110 DEG C
Under part, its viscosity remains to maintain original 70-80%, it is ensured that it has the term of validity long.Accelerated by auxiliary agent
Partially hydrolyzed polyacrylamide (PHPA) and the reaction speed of phenol-formaldehyde resin modified, make the high temperature resistant Weak Gels type profile control agent
Preparation it is more quick.It can be seen that, high temperature resistant Weak Gels type profile control agent provided in an embodiment of the present invention can be resistant to
90-110 DEG C of high temperature, and the term of validity is long, preparation method simple and fast, is easy to large-scale promotion application.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below will be to embodiment of the present invention
It is described in further detail.
In a first aspect, the embodiment of the invention provides a kind of high temperature resistant Weak Gels type profile control agent, the profile control agent bag
Include：Partially hydrolyzed polyacrylamide (PHPA), phenol-formaldehyde resin modified, auxiliary agent and water.In the profile control agent, partial hydrolysis
The concentration of polyacrylamide be 0.8g/L-2.5g/L (such as 0.8,1.2,1.5,2.0,2.2,2.5g/L), change
Property phenolic resin concentration for 0.6g/L-2.0g/L (such as 0.6,1.0,1.4,1.6,2.0g/L), auxiliary agent
Concentration be 0.5g/L-2.0g/L (such as 0.5,0.8,1.2,1.6,2.0g/L).
Specifically, phenol-formaldehyde resin modified is prepared via a method which to obtain：
To phenol is added in reactor, 45-55 DEG C is heated to, base catalyst is then added while stirring, protected
After warm 10-30min, then formalin is instilled, be rapidly heated to 70-90 DEG C, be incubated 3-5h, be eventually adding
Urea, 10-30min is incubated after being well mixed, and obtains phenol-formaldehyde resin modified.The mass concentration of formalin is
25-35%, phenol is 1 with the mol ratio of formaldehyde in formalin:2.7-3.3, amount of urea is phenol and formaldehyde
The 1-5% of solution gross mass.
Auxiliary agent is prepared via a method which to obtain：
Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is subsequently adding, is 6-8 in reaction system pH
And reacted under stirring, obtain auxiliary agent after finally sloughing moisture.Aluminium chloride, oxalic acid and ammonium chloride
Mol ratio be 1:(15-30):(70-90).
High temperature resistant Weak Gels type profile control agent provided in an embodiment of the present invention, using partially hydrolyzed polyacrylamide (PHPA) as
Host, is realized and host cross-linking reaction by phenol-formaldehyde resin modified, and under the complex role of auxiliary agent, institute's shape
Into high temperature resistant Weak Gels type profile control agent be resistant to 90-110 DEG C of high temperature, and the term of validity is long.Wherein, by changing
Property phenolic resin prepare during add urea, it is reacted with free formaldehyde, so as to reduce phenolic resin
In free formaldehyde, the profile control agent for obtaining is more environmentally-friendly, meanwhile, urea also acts as the effect of stabilizer, suppression
The decomposition of Weak Gels system processed, makes Weak Gels system plastic after 30 days, in the height that formation temperature is 90-110 DEG C
Under the conditions of temperature, its viscosity remains to maintain original 70-80%, it is ensured that it has the term of validity long.By auxiliary agent
Accelerate the reaction speed of partially hydrolyzed polyacrylamide (PHPA) and phenol-formaldehyde resin modified, adjust the high temperature resistant Weak Gels type
The preparation for cuing open agent is more quick.It can be seen that, high temperature resistant Weak Gels type profile control agent provided in an embodiment of the present invention can
Resistance to 90-110 DEG C of high temperature, and the term of validity is long, preparation method simple and fast, is easy to large-scale promotion application.
Second aspect, the embodiment of the present invention additionally provides a kind of side for preparing the high temperature resistant Weak Gels type profile control agent
Method, comprises the following steps：
Step 101, prepare phenol-formaldehyde resin modified
To phenol is added in reactor, 45-55 DEG C is heated to, such as 45 DEG C, 48 DEG C, 50 DEG C, 53 DEG C, 55 DEG C,
Then add base catalyst while stirring, after insulation 10-30min, such as insulation 10min, 15min, 20min,
25min, 30min, then instill formalin, are rapidly heated to 70-90 DEG C, such as 70 DEG C, 75 DEG C, 80 DEG C,
85 DEG C, 90 DEG C, insulation 3-5h, such as 3h, 4h, 5h obtain phenolic resin, are eventually adding urea, mix
Insulation 10-30min after uniform, such as 10min, 15min, 20min, 25min, 30min, are modified
Phenolic resin.
Wherein, the mass concentration of formalin is 25-35%, preferably 30%, first in phenol and formalin
The mol ratio of aldehyde is 1:2.7-3.3, such as 1:2.7、1:2.9、1:3.1、1:3.3, urea is phenol and formalin
The 1-5% of gross mass, such as 1%, 2%, 3%, 4%, 5%.Step 101 is by using urea to phenolic aldehyde tree
Fat is modified, and after urea reacts with free formaldehyde, reduces the free formaldehyde in phenolic resin, obtains more
The profile control agent of environmental protection, meanwhile, urea also acts as the effect of stabilizer, suppresses the decomposition of Weak Gels system, from
And the durability of the Weak Gels type profile control agent is improved, and make it after plastic 30 days, it is 90-110 DEG C in formation temperature
Hot conditions under, its viscosity remains to maintain original 70-80%, so that with the term of validity more long.
In high temperature resistant Weak Gels type profile control agent provided in an embodiment of the present invention, phenol-formaldehyde resin modified is used as crosslinking
Agent is used, and it can be in intermolecular bridging action of line style so that multiple linear molecules are mutually bonded and are cross-linked into net
Network structure, promotes or regulation polymer molecule interchain covalent bond or ionic bond are formed, make monomer in solution,
Linear macromolecule or prepolymer are transformed into the material of tridimensional network, that is, form Weak Gels system, so that right
High-permeability reservoir plays plugging action.Meanwhile, Weak Gels system has certain mobility again, can be in height
It is slow in permeability formation passage to be moved to earth formation deep, reach the effect of transfer drive.Therefore, the present invention is implemented
The high temperature resistant Weak Gels type profile control agent that example is provided has preferable profile control effect.
Specifically, the base catalyst used in step 101 is NaOH, and base catalyst can promote
Phenol and the reaction of formaldehyde, improve reaction rate.The consumption of base catalyst is formalin and the total matter of phenol
The 2-10% of amount, such as 2%, 5%, 8%, 10%.
Step 102, prepare auxiliary agent
Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is subsequently adding, is 6-8 in reaction system pH
And reacted under stirring, obtain auxiliary agent after finally sloughing moisture.Wherein, aluminium chloride, oxalic acid and
The mol ratio of ammonium chloride is 1:(15-30):(70-90), such as 1:15:70、1:23:80、1:30:90.
By above-mentioned auxiliary agent, phenol-formaldehyde resin modified can be accelerated with partially hydrolyzed polyacrylamide (PHPA) cross-linking reaction
Speed, improves hydroxyl and partially hydrolyzed polyacrylamide (PHPA) condensation ratio, and reacting fully is carried out.
Specifically, in step 102, the total time that instilling formalin needs is that 10-60min, i.e. formaldehyde are molten
Liquid should drip in 10-60min (such as 10min, 20min, 30min, 40min, 50min, 60min)
Add it is complete, to ensure that phenol and the reaction of formaldehyde are carried out completely.
Specifically, in step 102, when adjusting the pH of reaction system, can be adjusted using ammoniacal liquor,
Until the pH of reaction system is in the range of 6-8, it is ensured that auxiliary agent can improve the stability of auxiliary agent in neutrality,
The acid-base value of auxiliary agent is avoided to phenol-formaldehyde resin modified and the cross-linking reaction of partially hydrolyzed polyacrylamide (PHPA).
Step 103, preparation high temperature resistant Weak Gels type profile control agent
The aqueous solution of partially hydrolyzed polyacrylamide (PHPA) is prepared, then to the aqueous solution of partially hydrolyzed polyacrylamide (PHPA)
It is middle to add phenol-formaldehyde resin modified and auxiliary agent, it is well mixed and is put into climatic chamber, enter at 90-110 DEG C
The treatment of row constant temperature, obtains high temperature resistant Weak Gels type profile control agent.In high temperature resistant Weak Gels type profile control agent, part water
Solve polyacrylamide concentration for 0.8g/L-2.5g/L (such as 0.8,1.2,1.5,2.0,2.2,2.5g/L),
The concentration of phenol-formaldehyde resin modified be 0.6g/L-2.0g/L (such as 0.6,1.0,1.4,1.6,2.0g/L), auxiliary agent
Concentration for 0.5g/L-2.0g/L (such as 0.5,0.8,1.2,1.6,2.0g/L).Phenol-formaldehyde resin modified it is dense
It is 0.6g/L-2.0g/L to spend, and the concentration of auxiliary agent is 0.5g/L-2.0g/L.
Specifically, in step 103, constant temperature process time be 8-40h, such as 8h, 10h, 15h, 20h, 25h,
30h, 35h, 40h etc., the relative air humidity of climatic chamber is 1-3%, such as 1%, 2%, 3%, with
Maintenance reaction speed.Product is formed Weak Gels, and with certain humidity, be adapted to be present in 90-110 DEG C
Ground environment in.
Specifically, in step 103, the aqueous solution for preparing partially hydrolyzed polyacrylamide (PHPA) includes：By part water
Solution polyacrylamide is slowly added in water, and is suitably stirred, it is to avoid consolidation, and stirring should not be too violent,
In order to avoid cause depolymerization, influence using effect, stirring curing is advisable with 2-4h, such as 2h, 2.5h, 3h,
3.5h、4h.Obtain the aqueous solution of partially hydrolyzed polyacrylamide (PHPA).Use the partial hydrolysis polypropylene of Fresh
The aqueous solution of acid amides, it is to avoid its performance is gradually reduced with the extension of the situation and time of water quality.
Hereinafter will further be elaborated by specific embodiment：
Embodiment 1
The present embodiment is prepared to phenol-formaldehyde resin modified and auxiliary agent used in profile control agent first, specifically
It is as follows：
1) phenol-formaldehyde resin modified, is prepared
To the phenol that 18.0g is added in reactor, 50 DEG C are heated to, 3.6g mass is then added while stirring
Concentration be 10% NaOH as catalyst.After insulation 10min, 18g mass is added dropwise in 35min dense
The formalin for 30% is spent, is rapidly heated to 70 DEG C, be incubated 3h.4g urea is eventually adding, mixing is equal
Insulation 10min, is cooled to room temperature after even, obtains phenol-formaldehyde resin modified.
2) auxiliary agent, is prepared
Water dissolves are used after 1.34g aluminium chloride is mixed with 18g oxalic acid, 42.76g ammonium chlorides are subsequently adding, stirred
Mix uniform, adjusting reaction system pH with ammoniacal liquor is about 7, and moisture is sloughed after reaction, obtains auxiliary agent.
3) aqueous solution of fresh partially hydrolyzed polyacrylamide (PHPA) is prepared
Embodiment 2
Phenol-formaldehyde resin modified that the present embodiment provides embodiment 1, auxiliary agent, partially hydrolyzed polyacrylamide (PHPA)
The aqueous solution is well mixed, and is put into climatic chamber, is carried out under conditions of 90 DEG C, relative humidity are for 1%
Constant temperature treatment, obtains high temperature resistant Weak Gels type profile control agent.Wherein, it is each in the high temperature resistant Weak Gels type profile control agent
The content of component is as follows：
Partially hydrolyzed polyacrylamide (PHPA) concentration is 0.8g/L, and modified phenolic resin lipid concentration is 0.6g/L, and auxiliary agent is dense
It is 0.5g/L to spend.
The initial viscosity of the high temperature resistant Weak Gels type profile control agent to preparing is measured, and is 1223mPas,
It is subsequently placed in tool plug wide-mouth bottle, observes plastic situation, after is placed 30 days in wide-mouth bottle, then to this
The viscosity of profile control agent is measured, and is 966mPas, it is seen then that high temperature resistant Weak Gels obtained in the present embodiment
Type profile control agent works well.
Embodiment 3
Phenol-formaldehyde resin modified that the present embodiment provides embodiment 1, auxiliary agent, partially hydrolyzed polyacrylamide (PHPA)
The aqueous solution is well mixed, and is put into climatic chamber, is carried out under conditions of 110 DEG C, relative humidity 2%
Constant temperature treatment, obtains high temperature resistant Weak Gels type profile control agent.Wherein, it is each in the high temperature resistant Weak Gels type profile control agent
The content of component is as follows：
Partially hydrolyzed polyacrylamide (PHPA) concentration is 2.5g/L, and modified phenolic resin lipid concentration is 2.0g/L, assistant concentration
It is 2.0g/L.
The initial viscosity of the high temperature resistant Weak Gels type profile control agent to preparing is measured, and is 1857mPas,
It is subsequently placed in tool plug wide-mouth bottle, observes plastic situation, after is placed 30 days in wide-mouth bottle, then to this
The viscosity of profile control agent is measured, and is 1318mPas, it is seen then that high temperature resistant Weak Gels obtained in the present embodiment
Type profile control agent works well.
Embodiment 4
Phenol-formaldehyde resin modified that the present embodiment provides embodiment 1, auxiliary agent, partially hydrolyzed polyacrylamide (PHPA)
The aqueous solution is well mixed, and is put into climatic chamber, is carried out under conditions of 100 DEG C, relative humidity 3%
Constant temperature treatment, obtains high temperature resistant Weak Gels type profile control agent.Wherein, it is each in the high temperature resistant Weak Gels type profile control agent
The content of component is as follows：
Partially hydrolyzed polyacrylamide (PHPA) concentration is 1.7g/L, and modified phenolic resin lipid concentration is 1.3g/L, assistant concentration
1.2g/L。
The initial viscosity of the high temperature resistant Weak Gels type profile control agent to preparing is measured, and is 1682mPas,
It is subsequently placed in tool plug wide-mouth bottle, observes plastic situation, after is placed 30 days in wide-mouth bottle, then to this
The viscosity of profile control agent is measured, and is 1228mPas, it is seen then that high temperature resistant Weak Gels obtained in the present embodiment
Type profile control agent works well.
Presently preferred embodiments of the present invention is the foregoing is only, the protection domain being not intended to limit the invention is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc., all should include
Within protection scope of the present invention.
Claims (9)
1. a kind of high temperature resistant Weak Gels type profile control agent, including：Partially hydrolyzed polyacrylamide (PHPA), phenol-formaldehyde resin modified, auxiliary agent and water；The partially hydrolyzed polyacrylamide (PHPA) concentration is 0.8g/L-2.5g/L, and the modified phenolic resin lipid concentration is 0.6g/L-2.0g/L, and the assistant concentration is 0.5g/L-2.0g/L；
The phenol-formaldehyde resin modified is prepared via a method which to obtain：
To phenol is added in reactor, 45-55 DEG C is heated to, base catalyst is then added while stirring, after insulation 10-30min, formalin is instilled again, is rapidly heated to 70-90 DEG C, be incubated 3-5h, urea is eventually adding, 10-30min is incubated after being well mixed, obtain the phenol-formaldehyde resin modified；
The mass concentration of the formalin is 25-35%, and the phenol is 1 with the mol ratio of formaldehyde in the formalin:2.7-3.3, the amount of urea is the 1-5% of the phenol and the formalin gross mass；
The auxiliary agent is prepared via a method which to obtain：
Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is subsequently adding, is reacted in the case where reaction system pH is 6-8 and stirring, the auxiliary agent is obtained after finally sloughing moisture；
The mol ratio of the aluminium chloride, oxalic acid and ammonium chloride is 1:(15-30):(70-90).
2. the preparation method of the high temperature resistant Weak Gels type profile control agent described in claim 1, including：
Step a, prepare phenol-formaldehyde resin modified
To phenol is added in reactor, 45-55 DEG C is heated to, base catalyst is then added while stirring, after insulation 10-30min, formalin is instilled again, is rapidly heated to 70-90 DEG C, be incubated 3-5h, urea is eventually adding, 10-30min is incubated after being well mixed, obtain the phenol-formaldehyde resin modified；
The mass concentration of the formalin is 25-35%, and the phenol is 1 with the mol ratio of formaldehyde in the formalin:2.7-3.3, the urea is the 1-5% of the phenol and the formalin gross mass；
Step b, prepare auxiliary agent
Water dissolves are used after aluminium chloride is mixed with oxalic acid, ammonium chloride is subsequently adding, is reacted in the case where reaction system pH is 6-8 and stirring, the auxiliary agent is obtained after finally sloughing moisture；
The mol ratio of the aluminium chloride, oxalic acid and ammonium chloride is 1:(15-30):(70-90)；
Step c, preparation high temperature resistant Weak Gels type profile control agent
Prepare the aqueous solution of partially hydrolyzed polyacrylamide (PHPA), then to adding the phenol-formaldehyde resin modified and the auxiliary agent in the aqueous solution of the partially hydrolyzed polyacrylamide (PHPA), it is well mixed and is put into climatic chamber, constant temperature treatment is carried out at 90-110 DEG C, the high temperature resistant Weak Gels type profile control agent is obtained；
In the high temperature resistant Weak Gels type profile control agent, the concentration of the partially hydrolyzed polyacrylamide (PHPA) is 0.8g/L-2.5g/L, and the concentration of the phenol-formaldehyde resin modified is 0.6g/L-2.0g/L, and the concentration of the auxiliary agent is 0.5g/L-2.0g/L.
3. preparation method according to claim 2, it is characterised in that the base catalyst is NaOH.
4. preparation method according to claim 2, it is characterised in that the consumption of the base catalyst is the 2-10% of the formalin and the phenol gross mass.
5. preparation method according to claim 2, it is characterised in that in the step a, the total time that instilling the formalin needs is 10-60min.
6. preparation method according to claim 2, it is characterised in that in the step b, the pH that the reaction system is adjusted with ammoniacal liquor is 6-8.
7. preparation method according to claim 2, it is characterised in that in the step c, the constant temperature process time is 8-40h.
8. preparation method according to claim 2, it is characterised in that in the step c, the relative air humidity of the climatic chamber is 1-3%.
9. preparation method according to claim 2, it is characterised in that in the step c, the aqueous solution for preparing the partially hydrolyzed polyacrylamide (PHPA) includes：The partially hydrolyzed polyacrylamide (PHPA) is added to the water, stirring curing 2-4h obtains the aqueous solution of the partially hydrolyzed polyacrylamide (PHPA).
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| CN107699219A (en) * | 2017-10-25 | 2018-02-16 | 中国石油化工股份有限公司 | High temperature resistance and high strength gel adjusts stifled system and preparation method thereof |
| CN107903365A (en) * | 2017-10-31 | 2018-04-13 | 中国石油天然气股份有限公司 | A kind of urea phenolic resin crosslinking agent and its synthetic method |
| CN108841369A (en) * | 2018-07-02 | 2018-11-20 | 陕西科技大学 | A kind of preparation method of polyacrylamide Weak Gels |
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| CN108841369A (en) * | 2018-07-02 | 2018-11-20 | 陕西科技大学 | A kind of preparation method of polyacrylamide Weak Gels |
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| CN111087990A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | High-temperature-resistant gel plugging agent composition and preparation method and application thereof |
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| CN111088023B (en) * | 2018-10-23 | 2022-01-04 | 中国石油化工股份有限公司 | High-temperature-resistant polyacrylamide gel plugging agent and preparation method and application thereof |
| CN111087992B (en) * | 2018-10-23 | 2022-01-04 | 中国石油化工股份有限公司 | Gel plugging agent composition and preparation method and application thereof |
| CN111087996B (en) * | 2018-10-23 | 2022-07-12 | 中国石油化工股份有限公司 | High-temperature-resistant composite gel plugging agent and preparation method and application thereof |
| CN109401740A (en) * | 2018-12-24 | 2019-03-01 | 陕西明德石油科技有限公司 | Oil field composite modified resin is crosslinked strong gel water-plugging profile control agent |
| CN110724281A (en) * | 2019-10-22 | 2020-01-24 | 陕西科技大学 | Sulfonated partially hydrolyzed polyacrylamide weak gel and preparation method thereof |
| CN115725033A (en) * | 2021-08-31 | 2023-03-03 | 中国石油化工股份有限公司 | Preparation method of cross-linking agent for oil field, cross-linking agent and blocking agent for oil field, and preparation method and application of cross-linking agent and blocking agent |
| CN115725033B (en) * | 2021-08-31 | 2024-02-13 | 中国石油化工股份有限公司 | Preparation method of cross-linking agent for oil field, cross-linking agent and plugging agent for oil field, and preparation method and application thereof |
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