CN104293324B - A kind of ultra-high temperature drilling liquid fluid loss additive and preparation method thereof - Google Patents
A kind of ultra-high temperature drilling liquid fluid loss additive and preparation method thereof Download PDFInfo
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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Abstract
The present invention relates to a kind of ultra-high temperature drilling liquid fluid loss additives and preparation method thereof, especially superhigh temperature salt-water drilling fluid high temperature and pressure fluid loss additive and preparation method thereof, belong to water-soluble high-molecular material and be synthetically prepared technical field, certain time is reacted by sulfomethylation phenolic resin and formaldehyde, hydroxyalkyl aldehyde, aliphatic ketone or alicyclic ketone, sulphite, pyrosulfite at high temperature under high pressure and is obtained.The present invention can effectively control the high temperature and high pressure filter loss and rheological characteristic of salt-water drilling fluid, there is good compatibility with LP527, MP488 and SMC etc., high-temperature stability is good, without there is thickening phenomenon after aging at 220 DEG C, drilling fluid high-temperature high pressure filter loss can effectively be controlled less than 16mL, density reaches 2.32g/cm3When, still there is preferable rheological characteristic.Preparation process is easily controllable, and product can satisfy the needs of 220 DEG C of ultra-high temperature drilling liquid high temperature and high pressure filter loss control.
Description
Technical field:
The present invention relates to a kind of ultra-high temperature drilling liquid fluid loss additives and preparation method thereof, especially superhigh temperature salt-water drilling fluid
High temperature and pressure fluid loss additive and preparation method thereof belongs to water-soluble high-molecular material and is synthetically prepared technical field, more precisely,
Belong to oil field chemical preparation technical field.
Technical background:
With the increasing of Deep Oil And Gas Exploration exploration and development dynamics, drilling strata becomes increasingly complex.In general, well is deeper, well
Lower pressure and temperature can be higher, and drilling completion is faced difficult also just bigger.In the world all there is high temperature and pressure in many places
Stratum.The area that such as U.S., the North Sea have exploited, it is more than 200 DEG C that many reservoir pressures, which are more than 1OOMPa, bottom hole temperature (BHT),.At me
The land southwest Tarim of state, the NE Sichuan in Sichuan, grand celebration Xu family's defensive wall, all there is different journeys for South Sea Yingqiong basin of ocean etc.
The high temperature of degree, drilling well and complete well problem under high pressure.Sulfomethylation phenolic resin or sulfonated phenol formaldehyde resin (SMP) are that this field is existing
The common high temperature and pressure fluid loss additive in field, is a kind of anionic water-soluble polyelectrolyte, has very strong temperature-resistant anti-salt ability, product
Soluble easily in water for brown-red powder, aqueous solution is in alkalescent, and the filtrate reducer for drilling fluid as temperature-resistant anti-salt can be effectively
The high temperature and high pressure filter loss for reducing drilling fluid, " three sulphur drilling fluids " system can be prepared by being used in conjunction with SMC, SMT or SMK etc.,
It is one of ideal high temperature deep well drilling fluid system, production technology is highly developed.Sulfomethylation phenolic resin is using this
Field conventional method preparation, referring specifically to document: the design of drilling fluid chemicals and new product development, Shaanxi Xi'an: Northwest University
Publishing house, 2006:256-258.The country is directed to the needs of ultra-deep well drilling, has carried out some spies in terms of ultra-deep well drilling liquid
Rope, but needs are not met by comprehensive performance, the country has carried out ultra-high temperature drilling liquid system research thus, and use is resistant to high temperatures
The compatibilities such as polymer treatment agent and sulfonated phenol formaldehyde resin, sulfonated lignite, the stable fresh water and 4% of performance at available 220 DEG C
Brine drilling liquid system.Under 220 DEG C of high-temperatures, although SMP, as high temperature and pressure fluid loss additive, saline-alkaline tolerance is not able to satisfy
It needs, but in terms of molecular structure, SMP has the feasibility that its salt-resistance is improved by molecular modification.CN201210254900.X
A kind of fluid loss additive for boring fluid and preparation method thereof is disclosed, by phenol, formaldehyde, humate, pyrosulfite, anhydrous sodium
Sulfate single step reaction obtains sulfonated phenolic humic acid resin;In the presence of initiator, sulfonated phenolic humic acid resin again with hydrogen
The mixture progress graft copolymerization of sodium oxide molybdena, 2- acrylamide-2-methyl propane sulfonic, acrylamide, alkyl acrylamide, dries
Dry, crushing is to get sulfonated phenolic humic acid resin-alkenyl monomer graft copolymer.
But NaCl content is more than and using SMP as high temperature and pressure fluid loss additive, loses effective after 4% in the drilling fluid
The effect of high temperature and high pressure filter loss is controlled, and rheological characteristic is deteriorated, and the high temperature and pressure leak-off of system is made in the case where high saliferous
Amount control, if only using high-temperature resistant polymer fluid loss additive, must just be reached in lower range by improving its dosage, but
With the increase of polymer dosage, system liquid phase viscosity increases, but to the control of high density drilling fluid rheological characteristic bring it is unfavorable because
Element.
Summary of the invention:
It is an object of the invention to by modifying SMP, that is, pass through the aquation group of increase product, introduce new suction
The ultra-high temperature drilling liquid fluid loss additive of attached group synthesis salt resistance, can meet the peace under shaft bottom superhigh temperature and (sodium chloride) environment with high salt
The needs of full wellbore construction, can control rheological characteristic, suspension stability under water-base drilling fluid high-temperature and high-pressure conditions, effectively reduce
The high temperature and high pressure filter loss of salt-water drilling fluid.
A second object of the present invention is to provide the preparation methods of above-mentioned ultra-high temperature drilling liquid fluid loss additive.
Ultra-high temperature drilling liquid fluid loss additive of the present invention, by sulfomethylation phenolic resin and formaldehyde, hydroxyalkyl aldehyde, ketone, sulfurous
Hydrochlorate, pyrosulfite and water, reaction obtains at high temperature under high pressure, and wherein dosage of each component is as follows:
The preparation method of ultra-high temperature drilling liquid fluid loss additive of the present invention, comprising the following steps:
(1) by 35% sulfomethylation phenolic resin of mass fraction be added autoclave, start stirring, then according to the ratio according to
Secondary that water, formaldehyde, ketone, hydroxyalkyl aldehyde, pyrosulfite, sulphite are added into reaction kettle, raw material continues stirring 30 after adding
~60min seals reaction kettle, heating, in 70~90 DEG C, insulation reaction 0.5~1 hour;
(2) reach subsequent temperature of continuing rising to step (1) the resulting mixture reaction time, at 125~160 DEG C react 3~
12h;It is cooling after reaction time reaches, pressure release, discharging, by being spray-dried powdery product.
The use of the sulfomethylation phenolic resin and formaldehyde, hydroxyalkyl aldehyde, ketone, sulphite, pyrosulfite and water
Amount proportion are as follows:
The ketone is aliphatic ketone or alicyclic ketone, can be acetone, methyl ethyl ketone or cyclohexanone.
The hydroxyalkyl aldehyde be glycollic aldehyde, 3-HPA, 3- hydroxybutyraldehyde, 4- hydroxybutyraldehyde, 5- hydrogenation of hydroxypentylaldehyd,
5,5- dihydroxy valeral or parahydroxyben-zaldehyde.
The sulphite is sodium sulfite, potassium sulfite or ammonium sulfite.
The pyrosulfite is sodium pyrosulfite, potassium metabisulfite or ammonium pyrosulfite.
The beneficial effects of the present invention are:
1, by carrying out the reaction such as further sulfonation to sulfonated-pheno-formoldehyde resin, the preferably anti-height of anti-salt property is prepared
There is more sulfonic acid groups and aromatic ring group in warm high pressure fluid loss additive strand, can effectively control salt-water drilling fluid
High temperature and high pressure filter loss and rheological characteristic have good compatibility with LP527, MP488 and SMC etc., can satisfy superelevation thermohaline
The needs of aqueous drilling fluid high temperature and high pressure filter loss control.
2, the salt water of the compositions such as product of the present invention and LP527-1, MP488, high-temperature stabilizer and SMC and saturated brine drilling well
Liquid high-temperature stability is good, high temperature thickening does not occur, can effectively control drilling fluid high-temperature high pressure filter loss and be less than 16mL, close
Degree reaches 2.32g/cm3When, still there is preferable rheological characteristic.
Detailed description of the invention:
Fig. 1 is the influence of dressing agent and dressing agent dosage to modified outcome intrinsic viscosity;
Fig. 2 is influence of the dressing agent dosage to drilling fluid apparent viscosity, plastic viscosity and yield value;
Fig. 3 be dressing agent dosage at the beginning of drilling fluid handled by the present invention, the influence of egress;
Fig. 4 is influence of the dressing agent dosage to drilling fluid API filtration and high temperature and high pressure filter loss;
Fig. 5 is influence of the salt dosage to drilling fluid filtration handled by modified outcome, is measured after 220 DEG C/16h, wherein
Dressing agent dosage (1) -0, (2) -17%, (3) -23%, (4) -28%, (5) -33%;
Fig. 6 is that 1 sample of embodiment is sample 1, the infrared spectrogram with SMP;
Fig. 7 is the differential thermal analysis curve of sample 1.
Specific embodiment:
The present invention will be further described combined with specific embodiments below:
Embodiment 1:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 160 parts of formaldehyde, 100 parts of phenol, 35
Reaction kettles are added in part sodium pyrosulfite and 42 parts of sodium sulfites, are reacted at a certain temperature after a certain period of time, by being added portionwise
335 parts of (containing 50 parts first added) methods, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
Mix, then according to the ratio successively into reaction kettle be added 60 parts of water, 7 parts of formaldehyde, 22.5 parts of cyclohexanone, 32.5 parts of 3- hydroxybutyraldehydes,
18 parts of sodium pyrosulfites, 20.5 parts of sodium sulfites, raw material continue to stir 30min after adding, and seal reaction kettle, heat up, in 90 DEG C,
Insulation reaction 0.5 hour;Reaction time reaches subsequent temperature of continuing rising, reacts 10h at 145 DEG C;It is cooling after reaction time reaches,
Pressure release, discharging, by being spray-dried powdery product, the present embodiment sample is sample 1.
Embodiment 2:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 162 parts of formaldehyde, 100 parts of phenol,
Reaction kettle is added in 34.5 parts of sodium pyrosulfites and 47.5 parts of sodium sulfites, reacts at a certain temperature after a certain period of time, by dividing
It criticizes and 335 parts of (containing 50 parts first added) methods is added, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
It mixes, 75 parts of water, 2.5 parts of formaldehyde, 18 parts of methyl ethyl ketone, 36 parts of 4- hydroxybutyraldehydes, 22 is then successively added into reaction kettle according to the ratio
Part potassium metabisulfite, 25.5 parts of potassium sulfites, raw material continue to stir 40min after adding, and seal reaction kettle, and heating is protected in 90 DEG C
Temperature reaction 0.5 hour;Reaction time reaches subsequent temperature of continuing rising, reacts 12h at 125 DEG C;It is cooling after reaction time reaches, it lets out
Pressure, discharging, by being spray-dried powdery product, the present embodiment sample is sample 2.
Embodiment 3:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 160 parts of formaldehyde, 100 parts of phenol, 35
Reaction kettles are added in part sodium pyrosulfite and 42 parts of sodium sulfites, are reacted at a certain temperature after a certain period of time, by being added portionwise
335 parts of (containing 50 parts first added) methods, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
It mixes, 75 parts of water, 7 parts of formaldehyde, 27 parts of cyclohexanone, 32.5 parts of 5- hydrogenation of hydroxypentylaldehyd, 22 is then successively added into reaction kettle according to the ratio
Part ammonium pyrosulfite, 13 parts of ammonium sulfites, raw material continue to stir 50min after adding, and seal reaction kettle, and heating is kept the temperature in 70 DEG C
Reaction 1 hour;Reaction time reaches subsequent temperature of continuing rising, reacts 10h at 150 DEG C;Cooling after reaction time reaches, pressure release goes out
Material, by being spray-dried powdery product.
Embodiment 4:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 156.5 parts of formaldehyde, 100 parts of phenol,
Reaction kettle is added in 37.25 parts of sodium pyrosulfites and 35.5 parts of sodium sulfites, reacts at a certain temperature after a certain period of time, by dividing
It criticizes and 320 parts of (containing 50 parts first added) methods is added, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
It mixes, 50 parts of water, 7.5 parts of formaldehyde, 10 parts of acetone, 12.5 parts of 3-HPAs, 8.5 is then successively added into reaction kettle according to the ratio
Part sodium pyrosulfite, 20 parts of sodium sulfites, raw material continue to stir 60min after adding, and seal reaction kettle, and heating is kept the temperature in 70 DEG C
Reaction 1 hour;Reaction time reaches subsequent temperature of continuing rising, reacts 3h at 160 DEG C;Cooling after reaction time reaches, pressure release goes out
Material, by being spray-dried powdery product.
Embodiment 5:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 160 parts of formaldehyde, 100 parts of phenol, 35
Reaction kettles are added in part sodium pyrosulfite and 42 parts of sodium sulfites, are reacted at a certain temperature after a certain period of time, by being added portionwise
335 parts of (containing 50 parts first added) methods, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
Mix, then according to the ratio successively into reaction kettle be added 60 parts of water, 7 parts of formaldehyde, 20.5 parts of acetone, 32.5 parts of parahydroxyben-zaldehydes,
18 parts of sodium pyrosulfites, 20.5 parts of sodium sulfites, raw material continue to stir 60min after adding, and seal reaction kettle, heat up, in 80 DEG C,
Insulation reaction 45 minutes;Reaction time reaches subsequent temperature of continuing rising, reacts 7h at 150 DEG C;It is cooling after reaction time reaches, it lets out
Pressure, discharging, by being spray-dried powdery product.
Embodiment 6:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 160 parts of formaldehyde, 100 parts of phenol, 35
Reaction kettles are added in part sodium pyrosulfite and 42 parts of sodium sulfites, are reacted at a certain temperature after a certain period of time, by being added portionwise
335 parts of (containing 50 parts first added) methods, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
It mixes, 60 parts of water, 7 parts of formaldehyde, 22.5 parts of cyclohexanone, 32.5 parts of 5,5- dihydroxy penta is then successively added into reaction kettle according to the ratio
Aldehyde, 18 parts of sodium pyrosulfites, 20.5 parts of sodium sulfites, raw material continue to stir 45min after adding, and seal reaction kettle, heating, in 70
DEG C, insulation reaction 1 hour;Reaction time reaches subsequent temperature of continuing rising, reacts 5h at 160 DEG C;It is cooling after reaction time reaches,
Pressure release, discharging, by being spray-dried powdery product.
Embodiment 7:
Sulfonated-pheno-formoldehyde resin is prepared first, in accordance with literature method.By 50 parts of water, 160 parts of formaldehyde, 100 parts of phenol, 35
Reaction kettles are added in part sodium pyrosulfite and 42 parts of sodium sulfites, are reacted at a certain temperature after a certain period of time, by being added portionwise
335 parts of (containing 50 parts first added) methods, control the extent of reaction.
Autoclave is added in the 35% sulfomethylation phenolic resin of mass fraction of 625 parts of steps (1) preparation, starts and stirs
It mixes, 60 parts of water, 7 parts of formaldehyde, 22.5 parts of cyclohexanone, 28.5 parts of glycollic aldehydes, 18 is then successively added into reaction kettle according to the ratio
Part sodium pyrosulfite, 20.5 parts of sodium sulfites, raw material continue to stir 50min after adding, and seal reaction kettle, and heating is protected in 70 DEG C
Temperature reaction 1 hour;Reaction time reaches subsequent temperature of continuing rising, reacts 5h at 160 DEG C;It is cooling after reaction time reaches, pressure release,
Discharging, by being spray-dried powdery product.
The performance evaluation of experimental result of the invention is as follows:
Raw material except sulfonated-pheno-formoldehyde resin is known as dressing agent, wherein dressing agent 1 is by formaldehyde: 3- hydroxybutyraldehyde: ring
Hexanone: sodium sulfite: sodium pyrosulfite=1:6.5:4:3.5:3 ratio (mass ratio) composition;Dressing agent 2 is by formaldehyde: 5- hydroxyl penta
Aldehyde: acetone: sodium sulfite: sodium pyrosulfite=1:6.5:4.5:3.5:3 (mass ratio) composition.Dressing agent dosage is to account for dressing agent
With the mass fraction of sulfonated-pheno-formoldehyde resin gross mass.
1, the influence of different modifying agent and dosage to product intrinsic viscosity
Fig. 1 is the influence of dressing agent and dressing agent dosage to modified outcome intrinsic viscosity.It will be seen from figure 1 that using not
Same dressing agent influences difference to product intrinsic viscosity, and for dressing agent 1, with the increase of dressing agent dosage, gained modification is produced
The intrinsic viscosity of object gradually decreases, and when one timing of dressing agent dosage, reduction eases up, and when use dressing agent 2, the spy of modified outcome
Property viscosity number first improved with the increase of dressing agent dosage after again reduce.It is said in terms of ultra-high temperature drilling liquid is to the requirement of inorganic agent,
It is relatively good that salt resistance high temperature and pressure fluid loss additive is synthesized with dressing agent 1.
2, influence of the dressing agent to product property of drilling fluid
The basic recipe of drilling fluid used in the survey are as follows: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+
6%SMC+7% modified outcome+0.5%XJ+0.75%NaOH+10%NaCl is weighed out to density 2.3g/cm with barite3.It will
Then prepared drilling fluid is cooled to 55 DEG C and surveys its rheological characteristic in 220 DEG C of aging 16h, while measuring high temperature and high pressure filter loss
(180 DEG C, pressure difference 3.5MPa, similarly hereinafter) investigate the performance of product by high temperature and high pressure filter loss.
(1) influence of different modifying agent and dosage to property of drilling fluid handled by product
Fig. 2 is influence of the dressing agent dosage to drilling fluid apparent viscosity, plastic viscosity and yield value.It can from figure
Out, with the increase of dressing agent dosage, apparent viscosity, the plastic viscosity of drilling fluid handled by product are gradually decreased, for repairing
The product that agent 2 synthesizes is adornd, after dressing agent dosage is more than 28%, apparent viscosity and plastic viscosity increase again.And use gained
The yield value of drilling fluid handled by product is gradually decreased with the increase of dressing agent dosage, illustrates the production by modification from this point
Object can control drilling fluids at high temperature thickening phenomenon.
Fig. 3 be dressing agent dosage at the beginning of drilling fluid handled by product, the influence of egress.It can be seen from the figure that for repairing
Agent 1 is adornd, with the increase of dressing agent dosage, products therefrom ingressing for drilling fluid of processing is first reduced, and rear to increase again, egress first increases
Add, then reduces, it is rear to increase again.For dressing agent 2, with the increase of dressing agent dosage, products therefrom processing drilling fluid is ingressed
It gradually decreases, egress first increases, rear to reduce again.But total trend is with the increase of dressing agent dosage, the first of drilling fluid, egress
It reduces.
Fig. 4 is influence of the dressing agent dosage to drilling fluid API filtration and high temperature and high pressure filter loss.It can from figure
Out, dressing agent 1 is gradually decreased with the increase of dressing agent dosage with the filter loss of products therefrom processing drilling fluid, for
Dressing agent 2, with the increase of dressing agent dosage, the filter loss of drilling fluid first increases to be reduced afterwards.And the high temperature and pressure filter of drilling fluid
Vector is greatly lowered with the increase of dressing agent dosage, rises after dressing agent dosage is more than 23%, and slightly, in experiment item
17%~28% pair of control high temperature and high pressure filter loss of dressing agent dosage is more advantageous under part.
Apparent viscosity, plastic viscosity, yield value and first, egress and the high temperature for comprehensively considering drilling fluid handled by product are high
Filter pressing loss, dressing agent dosage is preferable in 23%~28% effect under experimental conditions, and uses 1 products therefrom performance of dressing agent
Better than dressing agent 2.
(2) influence of the salt dosage to property of drilling fluid handled by modified outcome
On the basis of condition experiment, dressing agent 1 is selected to carry out Product formation (embodiment 1), and investigates salt dosage to repairing
Adorn influence (the base slurry composition used: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6% of product property of drilling fluid
SMC+7% modified outcome+0.5%XJ+0.75%NaOH is weighed out to density 2.3g/cm with barite3), table 1 is salt dosage pair
The influence of modified outcome rheological characteristic, Fig. 5 are (220 DEG C/16h of influence of the salt dosage to drilling fluid filtration handled by modified outcome
It measures afterwards).
Influence of the 1 salt dosage of table to modified outcome drilling fluid rheology
Note: it is 1. measured at 55 DEG C;2. too thick can not measure.
As it can be seen from table 1 the salt-resistance of product can significantly be improved by introducing dressing agent in synthesis.From drilling fluid
Rheological characteristic sees that drilling fluid anti-salt property handled by the product (i.e. SMP) without dressing agent is poor, and high temperature thickening occurs, and draws
Enter obviously eliminate after dressing agent high temperature thickening phenomenon, and with the increase of dressing agent dosage, the viscosity of locating drilling fluid by
It gradually reduces, rheological characteristic is further improved.From the point of view of high temperature and high pressure filter loss, with the increase of dressing agent dosage, salt resistance energy
Power improves, and filter loss reduces, but after dressing agent dosage reaches a certain amount of, is further added by dressing agent dosage to filtrate reducing influential effect
Less.Under experimental conditions, it is contemplated that the production cost of product, dressing agent dosage both can be with guarantee systems 23%~28%
Rheological characteristic can guarantee that high temperature and high pressure filter loss is lower again.
3, influence of the addition of filtrate reducer to property of drilling fluid
Table 2 is the dosage of sample 1 and sample 2 synthesized by embodiment optimization of C/C composites to drilling fluid rheology handled by product
With the influence of filter loss.Its drilling fluid composition: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+0.5%
The NaCl+0.25% surfactant of XJ+3.0gNaOH+20% aggravates consistency 2.3g/cm with barite3, filter loss exists
It is measured after 220 DEG C/16h aging.
Influence of the 2 modified outcome dosage of table to drilling fluid rheology handled by product
Note: it is 1. measured at 55 DEG C;2. too thick can not measure.
It can be seen that the increase with fluid loss additive sample dosage from Fig. 5 and table 2, filter loss is substantially reduced, when dosage is
The high temperature and high pressure filter loss of system can be controlled within 15ml when 7%, and drilling fluid rheology is further after high temperature
Improved, illustrates that the thinking of synthesizing high temperature high pressure fluid loss additive of the present invention is feasible.
4, Experiment of Compatibility
In order to further investigate designed adaptability of the product in drilling fluid, HSP table (is used using product of the invention
Show) the brine drilling formula of liquid of four groups of difference salt contents is designed with LP527, MP488, SMC, high-temperature stabilizer etc.:
No. 1: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+7%HTASP+0.5%XJ+
0.75%NaOH+0.1% surfactant+10%NaCl, is weighed out to 2.3g/cm with barite3;
No. 2: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+7%HTASP+0.5%XJ+
0.85%NaOH+0.1% surfactant+20%NaCl, is weighed out to 2.3g/cm with barite3;
No. 3: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+9%HTASP+0.5%XJ+1%
NaOH+0.1% surfactant+25%NaCl, is weighed out to 2.3g/cm with barite3;
No. 4: 2% sodium bentonites starch+2.75% stabilizer+1.0%LP527+3.5%MP488+6%SMC+6%HTASP+
0.5%XJ+1%NaOH+0.1% surfactant+36%NaCl, is weighed out to 2.1g/cm with barite3。
Drilling fluid, and the aging 16h at 220 DEG C are prepared according to four group of formula above, property of drilling fluid is measured, the results are shown in Table
3。
3 different formulations property of drilling fluid of table
From table 3 it is observed that the drilling fluid of four kinds of different formulations all has good rheological characteristic, high temperature and high pressure filter loss
≤ 16ml.Illustrate that system has good high-temperature stability, while also further illustrating that HTASP can effectively control salt water
Drilling fluid high-temperature high pressure filter loss.
5, infrared spectroscopy and heat analysis
(1) wave spectrum shows and finds out from Fig. 6, and the infrared spectrogram of sample 1 and SMP have apparent difference, and sample 1 occurs
New obvious absorption peaks.Wave number 3403,995cm-1Nearby there are the characteristic absorption of hydroxyl, wave number 1190,1043cm-1Nearby there is sulphur
The characteristic absorption of acidic group has the characteristic absorption of methyl or methylene near wave number 2931,2875,1444, wave number 3040,
1613、1512、1482、833cm-1Nearby there is the characteristic absorption of aromatic ring, to prove there is hydroxyl, sulfonic group in synthesis of product molecules
With the groups such as alkyl, more sulfonic groups and hydroxyl group are introduced compared with SMP in synthesis of product molecules of the present invention.
(2) from figure 7 it can be seen that polymer starts to decompose when temperature rises to 260 DEG C, thermal decomposition process can divide two
A stage: the first stage occurs between 311~729 DEG C, opposite with the thermal decomposition of methylol, sulfonic group and amido in side group
It answers, the temperature section at 729 DEG C or more occurs for second stage, and main polymer chain starts to decompose at this time, it is seen then that product is with higher
Thermal stability.
Claims (2)
1. a kind of ultra-high temperature drilling liquid fluid loss additive preparation method, characterized in that the following steps are included:
(1) by 35% sulfomethylation phenolic resin of mass fraction be added autoclave, start stirring, then according to the ratio successively to
In reaction kettle be added water, formaldehyde, ketone, hydroxyalkyl aldehyde, pyrosulfite, sulphite, raw material continue after adding stirring 30~
60min seals reaction kettle, heating, in 70~90 DEG C, insulation reaction 0.5~1 hour;
(2) reach subsequent temperature of continuing rising to step (1) the resulting mixture reaction time, 3~12h is reacted at 125~160 DEG C;
It is cooling after reaction time reaches, pressure release, discharging, by being spray-dried powdery product;
The dosage of the sulfomethylation phenolic resin and formaldehyde, hydroxyalkyl aldehyde, ketone, sulphite, pyrosulfite and water is matched
Than are as follows:
625 parts of the sulfomethylation phenolic resin of mass fraction 35%,
2.5~7.5 parts of the formaldehyde of mass fraction 37%,
12.5~36 parts of hydroxyalkyl aldehyde,
10~27 parts of ketone,
13~25.5 parts of sulphite,
8.5~22 parts of pyrosulfite,
50~75 parts of water;
The ketone is acetone, methyl ethyl ketone or cyclohexanone;
The hydroxyalkyl aldehyde be glycollic aldehyde, 3-HPA, 3- hydroxybutyraldehyde, 4- hydroxybutyraldehyde, 5- hydrogenation of hydroxypentylaldehyd, 5,5-
Dihydroxy valeral or parahydroxyben-zaldehyde.
2. the preparation method of ultra-high temperature drilling liquid fluid loss additive according to claim 1, characterized in that the sulfurous acid
Salt is sodium sulfite, potassium sulfite or ammonium sulfite;The pyrosulfite is sodium pyrosulfite, potassium metabisulfite or burnt sub-
Ammonium sulfate.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811355658.9A CN109401736B (en) | 2014-05-30 | 2014-05-30 | Ultra-temperature drilling fluid filtrate reducer |
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