CN106566490B - A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure and preparation method thereof - Google Patents
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure and preparation method thereof Download PDFInfo
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- 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
- 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
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
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Abstract
The present invention relates to a kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure and preparation method thereof.First, by the unsaturated monomer of hydroxyl, alkylol, phosphorus pentoxide and oil-soluble unsaturated monomer, in the presence of initiator, it is esterified and polymerisation, obtain the mixture of alkyl phosphate and the polymer with phosphate ester structure, then, by using aluminium salt as crosslinking agent the phosphate in mixture is carried out coordination cross-linked and obtains the oil base drilling fluid extracting and cutting agent with aluminium phosphate structure.The molecular weight of polymers compositions is controllable in the extracting and cutting agent, forms intermolecular net structure by the strong coordination cross-linked effect of the phosphate in molecule and aluminium salt, the dosage of product is small, carries and cuts excellent effect, and the influence to drilling fluid plastic viscosity is smaller.
Description
Technical field
The present invention relates to a kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure and preparation method thereof, belong to brill
Well chemistry and field of engineering technology.
Background technology
Oil base drilling fluid is in wellbore stability, lubrication anti-sticking, the expansion of suppression Shale Hydration and stratum pulping, and fast drilling
Etc. have a clear superiority, it has also become probing high temperature deep well, high-inclination directional well, horizontal well, offshore drilling, various complicated bore
The important means of well section and reservoir protection.Oil base drilling fluid generally existing viscosity is higher and deficiency that shear force is relatively low so that oil base
Drilling fluid suspension is poor, is unfavorable for the preparation of suspension drilling cuttings, weighting material and VHD oil base drilling fluid, and in oil base
During drilling fluid use, it has been found that under conditions of needing to control plastic viscosity, the raising of shear force is very difficult.Therefore,
Shear force is one of the crucial rheological parameter for determining oil base drilling fluid performance, directly influences that to take rock, anti-settling, equivalent circulation close
Degree, excitement and swabbing pressure etc., only suitable control shear force simultaneously keep stable, could successfully drill Holes of Complicated Wells.
Chinese patent literature CN105038734A discloses a kind of oil base drilling fluid extracting and cutting agent and preparation method thereof, described
Extracting and cutting agent is prepared by the raw material of following percentage by weight:50%~80% solvent, 15%~35% myristic acid,
5%~15% stearate, the raw material stir 1h, are cooled to normal temperature in 60~70 DEG C, complete oil base drilling fluid and are cut with carrying
The preparation of agent.This extracting and cutting agent for being prepared of invention is small to the viscosity influence of oil base drilling fluid, and formula is easy, heat-resisting property compared with
It is good.
Chinese patent literature CN105623625A discloses a kind of oil base drilling fluid extracting and cutting agent and preparation method thereof.The side
Method comprises the following steps:Maleic anhydride and styrene carry out polymerisation in the presence of solvent and initiator and mixed
Thing;Obtained mixture reacts in the presence of alcohol compound and catalyst obtains extracting and cutting agent crude product;Obtained extracting and cutting agent is thick
Product crush after removing organic solvent, drying, produce described oil base drilling fluid extracting and cutting agent.The extracting and cutting agent of this invention synthesis both had
Long linear alkyl simultaneously contains substantial amounts of polar group, and chain alkyl forms netted knot in oil base drilling fluid by association
Structure, and molecule polar groups are interacted by electrostatic attraction or hydrogen bond with other groups, form big netted of specific surface area
Structure, effectively raise the yield value of drilling fluid.
But the interaction between above-mentioned extracting and cutting agent molecule using Van der Waals force, hydrogen bond equimolecular Interaction Force as
Main, the intensity of these active forces is well below the intensity of Coordinative Chemistry key, and therefore, effect one is cut in carrying for such extracting and cutting agent product
As, it is difficult to play a part of " carry cutting and do not viscosify ".
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure
And preparation method thereof.An object of the present invention, which is to provide a kind of plastic viscosity on system, to be influenceed smaller, is carried and is cut positive effect,
Good with other additive for drilling fluid compatibilities, raw material sources are wide, the extracting and cutting agent that molecular weight is easily controlled;The second purpose is to provide conjunction
Into simple for process, high conversion rate, the simple preparation method of product postprocessing.
Technical scheme is as follows:
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
1~100,000;The extracting and cutting agent is that phosphate compound and aluminium salt are reacted to the product that 1~5h is obtained at 50~80 DEG C.
A kind of preparation method of the oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, including step are as follows:
(1) synthesis of phosphate compound
The unsaturated monomer of hydroxyl, alkylol, oil-soluble unsaturated monomer are mixed, stirred at 30~50 DEG C to molten
Melt;Inert atmosphere, under stirring condition, phosphorus pentoxide and initiator are added, obtains reaction solution;At 50~100 DEG C reaction 2~
10h, obtain the mixture of alkyl phosphate and the polymer with phosphate ester structure;
The unsaturated monomer of the hydroxyl is N hydroxymethyl acrylamide, N- hydroxyethyl acrylamides, acrylic acid hydroxyl second
One or more kinds of mixtures in ester or hydroxyethyl methacrylate;The oil-soluble unsaturated monomer is benzene second
Alkene, caprolactam, acrylic acid hexyl ester, acrylic acid octyl group ester, decyl acrylate, dodecylacrylate, third
One or more kinds of mixtures in olefin(e) acid cetyl ester or octadecyl acrylate;
(2) preparation of oil base drilling fluid extracting and cutting agent
The mixture for taking step (1) to obtain, stirring is to melting at 50~60 DEG C;Under stirring condition, aluminium salt is added, must be mixed
Liquid;The pH value for adjusting mixed liquor is 7~10, and 1~5h is reacted at 50~80 DEG C;Through drying, crush, obtain oil base drilling fluid with carrying
Cut agent.
, according to the invention it is preferred to, the mass concentration of the unsaturated monomer of hydroxyl is 20 in step (1) reaction solution
~50g/L, the mass concentration of alkylol is 500~800g/L, and the mass concentration of oil-soluble unsaturated monomer is 150~300g/
L, the mass concentration of phosphorus pentoxide is 50~160g/L, and the mass concentration of initiator is 0.1~5g/L.
, according to the invention it is preferred to, alkylol is hexanol, octanol, lauryl alcohol, hexadecanol or 18 in the step (1)
Mixture more than one or both of alcohol.
, according to the invention it is preferred to, initiator is azodiisobutyronitrile, ABVN, azo in the step (1)
Dicyclohexyl formonitrile HCN, dibenzoyl peroxide, the peroxidating trimethylacetic acid tert-butyl ester or di-cyclohexylperoxy di-carbonate.
, according to the invention it is preferred to, reaction temperature is 50~80 DEG C in the step (1), and the reaction time is 3~6h.
, according to the invention it is preferred to, inert atmosphere is nitrogen, argon gas or helium atmosphere in the step (1).
, according to the invention it is preferred to, the mass concentration of aluminium salt is 40~120g/L in step (2) mixed liquor.
, according to the invention it is preferred to, aluminium salt is aluminium chloride, aluminum nitrate or aluminum sulfate in the step (2).
, according to the invention it is preferred to, with the pH value of ammoniacal liquor regulation mixed solution in the step (2);Preferably, the step
Suddenly the pH value of regulation mixed solution is 7.5~9 in (2).
The principle of the present invention:
Oil base drilling fluid extracting and cutting agent prepared by the present invention has using carbon-carbon bond as main chain, hydrocarbon structure and phosphate ester structure
For the polymers compositions of side chain, the component oleophylic function admirable, can be well dissolved in oil phase;Chemical property is stable, tool
There is excellent heat-resisting property;Molecular size range is controllable, the plastic viscosity of system is influenceed smaller.Therefore, in oil phase, the polymerization
Thing component can be as the basic components for building intermolecular grid structure.Meanwhile contain aluminium ion component, these aluminium in extracting and cutting agent
Ion can form the structure of multinuclear aluminium ol bridge under suitable conditions, and the structure can form coordinate bond with multiple phosphates,
So as to play crosslink polymer molecules, the effect of intermolecular net structure is formed.The intensity of this coordination cross-linked effect is remote
The intermolecular force conventional more than Van der Waals force, hydrogen bond etc., meanwhile, its heat resistance is also better than conventional intermolecular interaction
Power.Therefore, this product show dosage is few, carry cut excellent effect, the feature that influences that small, heat resistance is excellent etc. on plastic viscosity.
The invention has the advantages that:
(1) the oil base drilling fluid extracting and cutting agent prepared by has the structure of aluminium phosphate, by the phosphate in molecule and
The strong coordination cross-linked effect of aluminium salt and form intermolecular net structure, the dosage of product is small, carries and cuts excellent effect.
(2) oil base drilling fluid prepared by is controllable with the molecular weight of polymers compositions in extracting and cutting agent product, to system plasticity
The influence of viscosity is smaller.
(3) the oil base drilling fluid extracting and cutting agent and other additive for drilling fluid compatibilities prepared by are good.
(4) the oil base drilling fluid extracting and cutting agent prepared by has a network structure, and heat-resisting property is excellent.
(5) raw material sources of the oil base drilling fluid extracting and cutting agent prepared by are extensive, and cheap, preparation technology is simply easy to
Operation.
(6) oil base drilling fluid extracting and cutting agent prepared by it is safe to use, it is environmentally safe.
Above-mentioned various features show that the present invention is adapted to industrial production, and is with a wide range of applications.
Brief description of the drawings
Fig. 1 is the infared spectrum of oil base drilling fluid extracting and cutting agent prepared by embodiment 1.
Embodiment
With reference to specific embodiment, the present invention is described further, but not limited to this.
Experimental method described in following embodiments simultaneously, is conventional method unless otherwise specified;The reagent and material
Material, unless otherwise specified, is commercially obtained.
Embodiment 1
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
7.6 ten thousand.
Preparation process is as follows:
(1) synthesis of phosphate compound
23g N- hydroxyethyl acrylamides, 400g octadecyl alcolols, 95g styrene are added to equipped with agitator, logical nitrogen successively
In the wolf bottle of pipe and thermometer, it is placed in stirring in 50 DEG C of water bath with thermostatic control and, to melting, is slow added into the oxidations of 52g five two
Phosphorus, stir and be passed through nitrogen, add 1.5g azodiisobutyronitriles, stir to obtain reaction solution;And temperature is risen to 55 DEG C, the reaction time
For 4h, reaction terminating, the mixture of alkyl phosphate and the polymer with phosphate ester structure is obtained;
The mass concentration of N- hydroxyethyl acrylamides is 43g/L in the reaction solution, and the mass concentration of octadecyl alcolol is 756g/
L, the mass concentration of styrene are 180g/L, and the mass concentration of phosphorus pentoxide is 98g/L, the mass concentration of azodiisobutyronitrile
For 2.8g/L.
(2) preparation of extracting and cutting agent
Mixture 300g in step (1) is taken in beaker, to be placed in stirring in 55 DEG C of waters bath with thermostatic control and extremely melt, stirring condition
Under, 30g aluminum nitrates are slowly added to, obtain mixed liquor;The mass concentration of aluminum nitrate is 98g/L in the mixed liquor;Adjusted again with ammoniacal liquor
The pH value for saving mixed liquor is 8.6, and system temperature risen into 60 DEG C, reaction time 2h, reaction terminating, product through drying, crush,
Obtain oil base drilling fluid extracting and cutting agent.
Fig. 1 is the infared spectrum of oil base drilling fluid extracting and cutting agent manufactured in the present embodiment.It will be seen from figure 1 that 857cm-1
For the characteristic absorption peak containing aluminium ion component, 724cm-1And 1467cm-1For the characteristic absorption peak of phenyl ring, 1083cm-1With
1221cm-1For the characteristic absorption peak of phosphate ester structure, 1579cm-1For the characteristic absorption peak of carbonyl, 2850cm-1And 2921cm-1For
The characteristic absorption peak of alkyl.As can be seen here, there is lipophilic polymer group by two-step reaction, gained oil base drilling fluid extracting and cutting agent
Point, bound phosphate groups and component containing aluminium ion.
Embodiment 2
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
3.7 ten thousand.
Preparation process such as embodiment 1, except that reaction temperature is 75 DEG C in step (1), reaction time 5h.
Embodiment 3
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
4.3 ten thousand.
Preparation process such as embodiment 1, except that alkylol is hexadecanol in step (1).
Embodiment 4
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
7.2 ten thousand.
Preparation process such as embodiment 1, except that step (1) oil-soluble monomer is octadecyl acrylate.
Embodiment 5
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
5.6 ten thousand.
Preparation process such as embodiment 1, except that aluminium salt is aluminium chloride in step (2), dosage 20g, the mixing
The mass concentration of aluminium chloride is 68g/L in liquid.
Embodiment 6
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
8.8 ten thousand.
Preparation process is as follows:
(1) synthesis of phosphate compound
10g N- hydroxyethyl acrylamides, 152g lauryl alcohols, 55g aliphatic acrylates are added to be equipped with and stirred successively
In the wolf bottle for mixing device, logical nitrogen pipe and thermometer, it is placed in stirring in 40 DEG C of waters bath with thermostatic control and, to melting, is slow added into 25g
Phosphorus pentoxide, stir and be passed through nitrogen, add 0.2g azodiisobutyronitriles, stir to obtain reaction solution;And temperature is risen to 50 DEG C,
Reaction time is 3h, reaction terminating, obtains the mixture of alkyl phosphate and the polymer with phosphate ester structure;
The mass concentration of N- hydroxyethyl acrylamides is 44g/L in the reaction solution, and the mass concentration of lauryl alcohol is 667g/
L, the mass concentration of aliphatic acrylate are 241g/L, and the mass concentration of phosphorus pentoxide is 110g/L, the isobutyl of azo two
The mass concentration of nitrile is 0.9g/L.
(2) preparation of extracting and cutting agent
Mixture 300g in step (1) is taken in beaker, to be placed in stirring in 50 DEG C of waters bath with thermostatic control and extremely melt, stirring condition
Under, 25g aluminum sulfate is slowly added to, obtains mixed liquor;The mass concentration of aluminum nitrate is 82g/L in the mixed liquor;Adjusted again with ammoniacal liquor
It is 7.5 to save system pH, system temperature is risen into 60 DEG C, reaction time 3h, reaction terminating, product obtains oily through drying, crushing
Base drilling fluid extracting and cutting agent.
Embodiment 7
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
1.8 ten thousand.
Preparation process is as follows:
(1) synthesis of phosphate compound
Successively by 35g hydroxy-ethyl acrylates, 550g octadecyl alcolols, 145g styrene be added to equipped with agitator, logical nitrogen pipe and
In the wolf bottle of thermometer, it is placed in stirring in 50 DEG C of waters bath with thermostatic control and, to melting, is slow added into 100g phosphorus pentoxides, stirs
Mix and be passed through nitrogen, add 3.5g azodiisobutyronitriles, stir to obtain reaction solution;And temperature is risen to 90 DEG C, reaction time 6h,
Reaction terminating, obtain the mixture of alkyl phosphate and the polymer with phosphate ester structure;
The mass concentration of hydroxy-ethyl acrylate is 46g/L in the reaction solution, and the mass concentration of octadecyl alcolol is 720g/L, benzene
The mass concentration of ethene is 189g/L, and the mass concentration of phosphorus pentoxide is 130g/L, and the mass concentration of azodiisobutyronitrile is
4.6g/L。
(2) preparation of extracting and cutting agent
Mixture 300g in step (1) is taken in beaker, to be placed in stirring in 60 DEG C of waters bath with thermostatic control and extremely melt, stirring condition
Under, 35g aluminium chloride is slowly added to, obtains mixed liquor;The mass concentration of aluminum nitrate is 114g/L in the mixed liquor;Adjusted again with ammoniacal liquor
It is 8.5 to save system pH, system temperature is risen into 80 DEG C, reaction time 5h, reaction terminating, product obtains oily through drying, crushing
Base drilling fluid extracting and cutting agent.
Embodiment 8
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
2.2 ten thousand.
Preparation process is as follows:
(1) synthesis of polymer
Successively by 25g N hydroxymethyl acrylamides, 420g hexadecanols, 100g dodecylacrylates, which are added to, to be equipped with
In the wolf bottle of agitator, logical nitrogen pipe and thermometer, it is placed in stirring in 45 DEG C of waters bath with thermostatic control and, to melting, is slow added into
70g phosphorus pentoxides, stir and be passed through nitrogen, add 2.5g azodiisobutyronitriles, stir to obtain reaction solution;And temperature is risen to 70
DEG C, reaction time 4h, reaction terminating, obtain the mixture of alkyl phosphate and the polymer with phosphate ester structure;
The mass concentration of N hydroxymethyl acrylamide is 43g/L in the reaction solution, and the mass concentration of hexadecanol is 728g/
L, the mass concentration of dodecylacrylate are 173g/L, and the mass concentration of phosphorus pentoxide is 121g/L, the isobutyl of azo two
The mass concentration of nitrile is 4.3g/L.
(2) preparation of extracting and cutting agent
Mixture 300g in step (1) is taken in beaker, to be placed in stirring in 50 DEG C of waters bath with thermostatic control and extremely melt, stirring condition
Under, 35g aluminium chloride is slowly added to, obtains mixed liquor;The mass concentration of aluminum nitrate is 112g/L in the mixed liquor;Adjusted again with ammoniacal liquor
It is 8 to save system pH, system temperature is risen into 65 DEG C, reaction time 3h, reaction terminating, product obtains oil base through drying, crushing
Drilling fluid extracting and cutting agent.
Embodiment 9
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
2.9 ten thousand.
Preparation process is as follows:
(1) synthesis of polymer
Successively by 10g hydroxyethyl methacrylates, 200g hexanols, 50g caprolactams be added to equipped with agitator,
In the wolf bottle of logical nitrogen pipe and thermometer, it is placed in stirring in 30 DEG C of waters bath with thermostatic control and, to melting, is slow added into 25g five and aoxidizes
Two phosphorus, stir and be passed through nitrogen, add 0.5g ABVNs, stir to obtain reaction solution;And temperature is risen to 100 DEG C, reaction
Time is 2h, reaction terminating, obtains the mixture of alkyl phosphate and the polymer with phosphate ester structure;
The mass concentration of hydroxyethyl methacrylate is 37g/L in the reaction solution, and the mass concentration of hexanol is 744g/L,
The mass concentration of caprolactam is 186g/L, and the mass concentration of phosphorus pentoxide is 93g/L, the matter of ABVN
Amount concentration is 1.9g/L.
(2) preparation of extracting and cutting agent
Mixture 300g in step (1) is taken in beaker, to be placed in stirring in 55 DEG C of waters bath with thermostatic control and extremely melt, stirring condition
Under, 20g aluminium chloride is slowly added to, obtains mixed liquor;The mass concentration of aluminum nitrate is 66g/L in the mixed liquor;Adjusted again with ammoniacal liquor
It is 9 to save system pH, system temperature is risen into 65 DEG C, reaction time 1h, reaction terminating, product obtains oil base through drying, crushing
Drilling fluid extracting and cutting agent.
Embodiment 10
A kind of oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, the extracting and cutting agent have aluminium phosphate structure,
The intermolecular effect by multinuclear ol bridge aluminium complex ion forms network structure;The molecular weight of polymers compositions is in the extracting and cutting agent
2.9 ten thousand.
Preparation process is as follows:
(1) synthesis of polymer
20g hydroxyethyl methacrylates, 300g octanols, 80g decyl acrylates are added to equipped with agitator, led to successively
In the wolf bottle of nitrogen pipe and thermometer, it is placed in stirring in 40 DEG C of waters bath with thermostatic control and, to melting, is slow added into the oxidations of 60g five two
Phosphorus, stir and be passed through nitrogen, add 2g dibenzoyl peroxides, stir to obtain reaction solution;And temperature is risen to 90 DEG C, the reaction time
For 10h, reaction terminating, the mixture of alkyl phosphate and the polymer with phosphate ester structure is obtained;
The mass concentration of hydroxyethyl methacrylate is 46g/L in the reaction solution, and the mass concentration of octanol is 695g/L,
The mass concentration of decyl acrylate is 185g/L, and the mass concentration of phosphorus pentoxide is 139g/L, dibenzoyl peroxide
Mass concentration is 4.6g/L.
(2) preparation of extracting and cutting agent
Mixture 300g in step (1) is taken in beaker, to be placed in stirring in 50 DEG C of waters bath with thermostatic control and extremely melt, stirring condition
Under, 30g aluminium chloride is slowly added to, obtains mixed liquor;The mass concentration of aluminum nitrate is 97g/L in the mixed liquor;Adjusted again with ammoniacal liquor
It is 9 to save system pH, system temperature is risen into 65 DEG C, reaction time 5h, reaction terminating, product obtains oil base through drying, crushing
Drilling fluid extracting and cutting agent.
Test example 1
Implement properties of product evaluation:
The oil base drilling fluid prepared as follows to the embodiment of the present invention 1~10 carries out performance test with extracting and cutting agent:
1st, test object:
Blank sample:The basic recipe of oil base drilling fluid is as follows:400mL 5# white oil+4g emulsifying agents+6gNa2CO3+ 8g is soaked
Agent+8g organoclay+125g barite+8g fluid loss additives.
Test specimens 1~10 are respectively the oil for adding in above-mentioned oil base drilling fluid and being prepared by the embodiment of the present invention 1~10 respectively
Base drilling fluid extracting and cutting agent, the addition quality of the extracting and cutting agent is 4g.
Comparative sample, come from domestic additive for drilling fluid manufacturer, trade mark FB-MOD.
2nd, method of testing:
Rheological property determines:
After test object high-speed stirred 20min, sealing 24h is conserved, and high-speed stirred 10min again after maintenance, surveys it
Rheological property.Then test object is fitted into ageing can the heat rolling 16h at 150 DEG C, 180 DEG C respectively, is cooled to room temperature, moves into
Agitator tank high speed stirs 5min, surveys its rheological property, is determined according to method specified in national standard GB/T16783.1-2006, and
Contrasted with comparative sample, determination data is referring to table 1.
The extracting and cutting agent Evaluation results of table 1
Comprehensive analysis, from data above, the oil base drilling fluid extracting and cutting agent that the present invention is prepared is relative to contrast
Sample plastic viscosity is small, yield value is big.Because there is no multinuclear aluminium ol bridge structure and stronger intermolecular net knot in comparative sample
Structure, and the extracting and cutting agent that the present invention is prepared has the structure of multinuclear aluminium ol bridge, the structure can be formed with multiple phosphates matches somebody with somebody
Position key, so as to play a part of crosslink polymer molecules, form intermolecular net structure, therefore the extracting and cutting agent is moulded to system
The influence of property viscosity is small, and yield value is big, carries and cuts that effect is good, and heat-resisting property is excellent.
Claims (9)
1. a kind of preparation method of the oil base drilling fluid extracting and cutting agent with aluminium phosphate structure, including step:
(1) synthesis of phosphate compound
The unsaturated monomer of hydroxyl, alkylol, oil-soluble unsaturated monomer are mixed, stirring extremely melting at 30~50 DEG C;It is lazy
Property atmosphere, under stirring condition, add phosphorus pentoxide and initiator, obtain reaction solution;2~10h is reacted at 50~100 DEG C, is obtained
Alkyl phosphate and with phosphate ester structure polymer mixture;
The unsaturated monomer of the hydroxyl be N hydroxymethyl acrylamide, N- hydroxyethyl acrylamides, hydroxy-ethyl acrylate or
One or more kinds of mixtures in hydroxyethyl methacrylate;The oil-soluble unsaturated monomer is styrene, second
Alkenyl caprolactam, acrylic acid hexyl ester, acrylic acid octyl group ester, decyl acrylate, dodecylacrylate, acrylic acid ten
One or more kinds of mixtures in six Arrcostabs or octadecyl acrylate;
(2) preparation of oil base drilling fluid extracting and cutting agent
The mixture for taking step (1) to obtain, stirring is to melting at 50~60 DEG C;Under stirring condition, aluminium salt is added, obtains mixed liquor;
The pH value for adjusting mixed liquor is 7~10, and 1~5h is reacted at 50~80 DEG C;Through drying, crush, obtain oil base drilling fluid and cut with carrying
Agent.
2. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is, the mass concentration of the unsaturated monomer of hydroxyl is 20~50g/L in step (1) reaction solution, the matter of alkylol
Amount concentration is 500~800g/L, and the mass concentration of oil-soluble unsaturated monomer is 150~300g/L, the quality of phosphorus pentoxide
Concentration is 50~160g/L, and the mass concentration of initiator is 0.1~5g/L.
3. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is that alkylol is more than one or both of hexanol, octanol, lauryl alcohol, hexadecanol or octadecyl alcolol in the step (1)
Mixture.
4. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is that initiator is azodiisobutyronitrile, ABVN, azo diisopropyl imidazoline hydrochloride, peroxidating in the step (1)
Dibenzoyl, the peroxidating trimethylacetic acid tert-butyl ester or di-cyclohexylperoxy di-carbonate.
5. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is that reaction temperature is 50~80 DEG C in the step (1), and the reaction time is 3~6h.
6. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is that inert atmosphere is nitrogen, argon gas or helium atmosphere in the step (1).
7. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is that the mass concentration of aluminium salt is 40~120g/L in step (2) mixed liquor.
8. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is that aluminium salt is aluminium chloride, aluminum nitrate or aluminum sulfate in the step (2).
9. the preparation method of the oil base drilling fluid extracting and cutting agent according to claim 1 with aluminium phosphate structure, it is special
Sign is, adjusts the pH value of mixed solution in the step (2) with ammoniacal liquor to 7.5~9.
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CN1258709A (en) * | 2000-01-13 | 2000-07-05 | 西安石油学院 | Oil-base aluminium phosphate gelatinizer for fracture liquid and its preparation |
WO2013043243A1 (en) * | 2011-09-19 | 2013-03-28 | Gupta, D.V. Satyanarayana | Compositions and methods of treating high temperature subterranean formations |
CN104232072A (en) * | 2013-06-21 | 2014-12-24 | 中国石油天然气股份有限公司 | Phosphate anhydrous fracturing fluid gelling agent and preparation and application thereof |
CN105176510A (en) * | 2015-09-06 | 2015-12-23 | 四川省贝特石油技术有限公司 | Preparation method of fracturing fluid for anhydrous organic temporary plugging turnaround fracturing |
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CN1258709A (en) * | 2000-01-13 | 2000-07-05 | 西安石油学院 | Oil-base aluminium phosphate gelatinizer for fracture liquid and its preparation |
WO2013043243A1 (en) * | 2011-09-19 | 2013-03-28 | Gupta, D.V. Satyanarayana | Compositions and methods of treating high temperature subterranean formations |
CN104232072A (en) * | 2013-06-21 | 2014-12-24 | 中国石油天然气股份有限公司 | Phosphate anhydrous fracturing fluid gelling agent and preparation and application thereof |
CN105176510A (en) * | 2015-09-06 | 2015-12-23 | 四川省贝特石油技术有限公司 | Preparation method of fracturing fluid for anhydrous organic temporary plugging turnaround fracturing |
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