CN104293324A - Ultrahigh-temperature drilling fluid filtrate reducer and its preparation method - Google Patents
Ultrahigh-temperature drilling fluid filtrate reducer and its preparation method Download PDFInfo
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Abstract
The invention relates to an ultrahigh-temperature drilling fluid filtrate reducer and its preparation method, especially relates to an ultrahigh-temperature brine drilling fluid high-temperature high-pressure filtrate reducer and its preparation method, and belongs to the technical field of synthesis of water-soluble polymer materials. The filtrate reducer is obtained through a reaction of sulfomethylated phenolic resin, formaldehyde, hydroxyalkyl aldehyde, alicyclic ketone or aliphatic ketone, sulfite and pyrosulfite at a high temperature under a high pressure for a certain time. The filtrate reducer can effectively control the high temperature and high pressure filtration loss and the rheological property of the brine drilling fluid, has good compatibility with LP527, MP488 and SMC, has good high temperature stability, has no thickening phenomenon after ageing at 220DEG C, can effectively control the high temperature and high pressure filtration loss of the drilling fluid less than 16 ml, and still has good rheological property under a density of 2.32 g/cm<3>. The preparation process is easy to control, and the above obtained product can satisfy the need of the control of the high temperature and high pressure filtration loss of the 220DEG C ultrahigh-temperature drilling fluid.
Description
Technical field:
The present invention relates to a kind of ultra-high temperature drilling liquid fluid loss agent and preparation method thereof, particularly ultrahigh-temperature salt-water drilling fluid High Temperature High Pressure fluid loss agent and preparation method thereof, belong to water-soluble high-molecular material synthesis preparing technical field, or rather, belong to oil field chemical preparing technical field.
Technical background:
Along with the increasing of Deep Oil And Gas Exploration exploratory development dynamics, drilling strata becomes increasingly complex.In general, well is darker, and down-hole pressure and temperature can be higher, and the difficulty that drilling completion faces is also just larger.All there is High Temperature High Pressure stratum in many places in the world.As the area that the U.S., the North Sea etc. have been exploited, a lot of reservoir pressure more than 1OOMPa, bottom temperature more than 200 DEG C.At southwest Tarim, the NE Sichuan in Sichuan, Xu family's defensive wall of grand celebration that China is land, the drilling and completion technology problem all under the high temperature of various degrees, high pressure such as the South Sea Yingqiong basin of ocean.Sulfomethylation resol or sulfonated phenol formaldehyde resin (SMP) are the High Temperature High Pressure fluid loss agents that scene, this area is commonly used, it is a kind of anionic water-soluble polyelectrolyte, there is very strong temperature resistant antisalt ability, product is brown-red powder, soluble in water, the aqueous solution is weakly alkaline, as the filtrate reducer for drilling fluid of temperature resistant antisalt, effectively can reduce the high temperature and high pre ssure filtration of drilling fluid, jointly use with SMC, SMT or SMK etc. and can prepare " three sulphur drilling fluids " system, be one of desirable high temperature deep well drilling fluid system, its production technique is very ripe.Sulfomethylation resol adopts this area ordinary method preparation, specifically see document: the design of drilling fluid chemical and new product development, Xi'an, Shaanxi: press of Northwest University, 2006:256-258.The domestic needs for ultra-deep well drilling, in ultra-deep well drilling liquid, carry out some explore, but can't satisfy the demand in over-all properties, for this reason domesticly carry out the research of ultra-high temperature drilling liquid system, adopt high-temperature resistant polymer treatment agent and the compatibility such as sulfonated phenol formaldehyde resin, sulfonated lignite, fresh water and the 4% DWSW liquid system of stable performance at 220 DEG C can be obtained.Under 220 DEG C of high-temperatures, although SMP is as High Temperature High Pressure fluid loss agent, its saline-alkaline tolerance can not be satisfied the demand, and from molecular structure, SMP has the feasibility being improved its salt resistance by molecular modification.CN201210254900.X discloses a kind of fluid loss additive for boring fluid and preparation method thereof, obtains sulfonated phenolic humic acid resin by phenol, formaldehyde, humate, pyrosulfite, anhydrous sodium vitriol single step reaction; Under initiator exists, sulfonated phenolic humic acid resin carries out graft copolymerization with the mixture of sodium hydroxide, 2-acrylamide-2-methyl propane sulfonic, acrylamide, alkyl acrylamide again, dry, pulverize, obtain sulfonated phenolic humic acid resin-alkenyl monomer graft copolymer.
But after NaCl content in drilling fluid is more than 4%, using SMP as High Temperature High Pressure fluid loss agent, lose the effect effectively controlling high temperature and high pre ssure filtration, and rheological is deteriorated, the high temperature and high pre ssure filtration of system will be made to control in lower scope when high saliferous, if only use high-temperature resistant polymer fluid loss agent, just must by improving its dosage to reach, but along with the increase of polymkeric substance dosage, system liquid phase viscosity increases, and to again high density drilling fluid rheological to control to bring unfavorable factor.
Summary of the invention:
The object of the invention is to by modifying SMP, namely by increase product aquation group, introduce the ultra-high temperature drilling liquid fluid loss agent that new adsorption group synthesizes anti-salt, the needs of the safety drilling construction under shaft bottom ultrahigh-temperature and high salt (sodium-chlor) environment can be met, rheological, suspension stability under water-base drilling fluid high-temperature and high-pressure conditions can be controlled, effectively reduce the high temperature and high pre ssure filtration of salt-water drilling fluid.
Second object of the present invention is to provide the preparation method of above-mentioned ultra-high temperature drilling liquid fluid loss agent.
Ultra-high temperature drilling liquid fluid loss agent of the present invention, by sulfomethylation resol and formaldehyde, hydroxyalkyl aldehyde, ketone, sulphite, pyrosulfite and water, be obtained by reacting at high temperature under high pressure, wherein each amounts of components is as follows:
The preparation method of ultra-high temperature drilling liquid fluid loss agent of the present invention, comprises the following steps:
(1) massfraction 35% sulfomethylation resol is added autoclave, start stirring, then in reactor, water, formaldehyde, ketone, hydroxyalkyl aldehyde, pyrosulfite, sulphite is added successively by proportioning, raw material adds rear continuation stirring 30 ~ 60min, sealed reactor, heat up, in 70 ~ 90 DEG C, insulation reaction 0.5 ~ 1 hour;
(2) treat that the mixture reaction time of step (1) gained reaches follow-up temperature of continuing rising, at 125 ~ 160 DEG C, react 3 ~ 12h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
The consumption proportion of described sulfomethylation resol and formaldehyde, hydroxyalkyl aldehyde, ketone, sulphite, pyrosulfite and water is:
Described ketone is aliphatic ketone or alicyclic ketone, can be acetone, methylethylketone or pimelinketone.
Described hydroxyalkyl aldehyde is glycollic aldehyde, 3-HPA, 3-acetaldol, 4-acetaldol, 5-hydrogenation of hydroxypentylaldehyd, 5,5-dihydroxyl valeral or p-Hydroxybenzaldehyde.
Described sulphite is S-WAT, potassium sulfite or ammonium sulphite.
Described pyrosulfite is Sodium Pyrosulfite, potassium pyrosulfite or ammonium pyrosulfite.
The invention has the beneficial effects as follows:
1, by carrying out the reactions such as further sulfonation to sulfonated-pheno-formoldehyde resin, prepare in anti-salt property good high temperature resistance high pressure drop fluid loss agents molecular chain and there is more sulfonic acid group and aromatic ring group, effectively can control high temperature and high pre ssure filtration and the rheological of salt-water drilling fluid, with LP527, MP488 and SMC etc., there is good compatibleness, the needs that ultrahigh-temperature salt-water drilling fluid high temperature and high pre ssure filtration controls can be met.
2, the salt solution that forms such as product of the present invention and LP527-1, MP488, high-temperature stabiliser and SMC and saturated salt-water drilling fluid high-temperature stability good, there is not high temperature multiviscosisty, effectively can control drilling fluid high-temperature high pressure filter loss and be less than 16mL, density reaches 2.32g/cm
3time, still there is good rheological.
Accompanying drawing illustrates:
Fig. 1 is that modifier and modifier consumption are on the impact of modified outcome intrinsic viscosity;
Fig. 2 is the impact of modifier consumption on drilling fluid apparent viscosity, plastic viscosity and yield value;
Fig. 3 is modifier consumption on drilling fluid handled by the present invention just, the impact of egress;
Fig. 4 is modifier consumption on the impact of drilling fluid API filtration and high temperature and high pre ssure filtration;
Fig. 5 is salt dosage on the impact of drilling fluid filtration handled by modified outcome, measures, wherein after 220 DEG C/16h, modifier consumption (1)-0, (2)-17%, (3)-23%, (4)-28%, (5)-33%;
Fig. 6 is embodiment 1 sample is sample 1, with the infrared spectrogram of SMP;
Fig. 7 is the differential thermal analysis curve of sample 1.
Embodiment:
Below in conjunction with specific embodiment, the present invention will be further described:
Embodiment 1:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 160 parts of formaldehyde, 100 parts of phenol, 35 parts of Sodium Pyrosulfites and 42 parts of S-WATs being added reactor, after reacting certain hour at a certain temperature, by adding 335 parts of (50 parts containing first adding) methods in batches, controlling level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then in reactor, 60 parts of water, 7 parts of formaldehyde, 22.5 parts of pimelinketone, 32.5 parts of 3-acetaldols, 18 parts of Sodium Pyrosulfites, 20.5 parts of S-WATs are added successively by proportioning, raw material adds rear continuation and stirs 30min, sealed reactor, heat up, in 90 DEG C, insulation reaction 0.5 hour; Reaction times reaches follow-up temperature of continuing rising, at 145 DEG C, react 10h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product, the present embodiment sample is sample 1.
Embodiment 2:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 162 parts of formaldehyde, 100 parts of phenol, 34.5 parts of Sodium Pyrosulfites and 47.5 parts of S-WATs are added reactor, after reacting certain hour at a certain temperature, by adding 335 parts of (50 parts containing first adding) methods in batches, control level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then in reactor, 75 parts of water, 2.5 parts of formaldehyde, 18 parts of methylethylketones, 36 parts of 4-acetaldols, 22 parts of potassium pyrosulfites, 25.5 parts of potassium sulfites are added successively by proportioning, raw material adds rear continuation and stirs 40min, sealed reactor, heat up, in 90 DEG C, insulation reaction 0.5 hour; Reaction times reaches follow-up temperature of continuing rising, at 125 DEG C, react 12h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product, the present embodiment sample is sample 2.
Embodiment 3:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 160 parts of formaldehyde, 100 parts of phenol, 35 parts of Sodium Pyrosulfites and 42 parts of S-WATs being added reactor, after reacting certain hour at a certain temperature, by adding 335 parts of (50 parts containing first adding) methods in batches, controlling level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then in reactor, 75 parts of water, 7 parts of formaldehyde, 27 parts of pimelinketone, 32.5 parts of 5-hydrogenation of hydroxypentylaldehyd, 22 parts of ammonium pyrosulfites, 13 parts of ammonium sulphites are added successively by proportioning, raw material adds rear continuation and stirs 50min, sealed reactor, heat up, in 70 DEG C, insulation reaction 1 hour; Reaction times reaches follow-up temperature of continuing rising, at 150 DEG C, react 10h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
Embodiment 4:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 156.5 parts of formaldehyde, 100 parts of phenol, 37.25 parts of Sodium Pyrosulfites and 35.5 parts of S-WATs are added reactor, after reacting certain hour at a certain temperature, by adding 320 parts of (50 parts containing first adding) methods in batches, control level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then in reactor, 50 parts of water, 7.5 parts of formaldehyde, 10 parts of acetone, 12.5 parts of 3-HPAs, 8.5 parts of Sodium Pyrosulfites, 20 parts of S-WATs are added successively by proportioning, raw material adds rear continuation and stirs 60min, sealed reactor, heat up, in 70 DEG C, insulation reaction 1 hour; Reaction times reaches follow-up temperature of continuing rising, at 160 DEG C, react 3h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
Embodiment 5:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 160 parts of formaldehyde, 100 parts of phenol, 35 parts of Sodium Pyrosulfites and 42 parts of S-WATs being added reactor, after reacting certain hour at a certain temperature, by adding 335 parts of (50 parts containing first adding) methods in batches, controlling level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then in reactor, 60 parts of water, 7 parts of formaldehyde, 20.5 parts of acetone, 32.5 parts of p-Hydroxybenzaldehydes, 18 parts of Sodium Pyrosulfites, 20.5 parts of S-WATs are added successively by proportioning, raw material adds rear continuation and stirs 60min, sealed reactor, heat up, in 80 DEG C, insulation reaction 45 minutes; Reaction times reaches follow-up temperature of continuing rising, at 150 DEG C, react 7h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
Embodiment 6:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 160 parts of formaldehyde, 100 parts of phenol, 35 parts of Sodium Pyrosulfites and 42 parts of S-WATs being added reactor, after reacting certain hour at a certain temperature, by adding 335 parts of (50 parts containing first adding) methods in batches, controlling level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then by proportioning add in reactor successively 60 parts of water, 7 parts of formaldehyde, 22.5 parts of pimelinketone, 32.5 part 5,5-dihydroxyl valeral, 18 parts of Sodium Pyrosulfites, 20.5 parts of S-WATs, raw material adds rear continuation and stirs 45min, sealed reactor, heats up, in 70 DEG C, insulation reaction 1 hour; Reaction times reaches follow-up temperature of continuing rising, at 160 DEG C, react 5h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
Embodiment 7:
First sulfonated-pheno-formoldehyde resin is prepared according to literature method.The water of 50 parts, 160 parts of formaldehyde, 100 parts of phenol, 35 parts of Sodium Pyrosulfites and 42 parts of S-WATs being added reactor, after reacting certain hour at a certain temperature, by adding 335 parts of (50 parts containing first adding) methods in batches, controlling level of response.
The massfraction 35% sulfomethylation resol 625 parts of steps (1) prepared adds autoclave, start stirring, then in reactor, 60 parts of water, 7 parts of formaldehyde, 22.5 parts of pimelinketone, 28.5 parts of glycollic aldehydes, 18 parts of Sodium Pyrosulfites, 20.5 parts of S-WATs are added successively by proportioning, raw material adds rear continuation and stirs 50min, sealed reactor, heat up, in 70 DEG C, insulation reaction 1 hour; Reaction times reaches follow-up temperature of continuing rising, at 160 DEG C, react 5h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
The performance evaluation of experimental result of the present invention is as follows:
Raw material outside sulfonated-pheno-formoldehyde resin is called modifier, and wherein modifier 1 is by formaldehyde: 3-acetaldol: pimelinketone: S-WAT: Sodium Pyrosulfite=1:6.5:4:3.5:3 ratio (mass ratio) forms; Modifier 2 is by formaldehyde: 5-hydroxyl valeral: acetone: S-WAT: Sodium Pyrosulfite=1:6.5:4.5:3.5:3 (mass ratio) forms.Modifier consumption is the massfraction accounting for modifier and sulfonated-pheno-formoldehyde resin total mass.
1, different modifying agent and consumption are on the impact of product intrinsic viscosity
Fig. 1 is that modifier and modifier consumption are on the impact of modified outcome intrinsic viscosity.As can be seen from Figure 1, adopt different modifiers different on product intrinsic viscosity impact, for modifier 1, along with the increase of modifier consumption, the intrinsic viscosity of gained modified outcome reduces gradually, and when modifier consumption one timing, reduction eases up, and when adopting modifier 2, the intrinsic viscosity of modified outcome along with the increase of modifier consumption first improve after reduce again.From the requirement aspect of ultra-high temperature drilling liquid to treatment agent, synthesize anti-salt High Temperature High Pressure fluid loss agent with modifier 1 relatively good.
2, modifier is on the impact of product property of drilling fluid
The basic recipe of drilling fluid used is in the survey: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+7% modified outcome+0.5%XJ+0.75%NaOH+10%NaCl, increases the weight of to density 2.3g/cm with barite
3.By prepared drilling fluid in 220 DEG C of aging 16h, be then cooled to 55 DEG C and survey its rheological, Simultaneously test high temperature and high pre ssure filtration (180 DEG C, pressure reduction 3.5MPa, lower same), the performance of product is investigated by high temperature and high pre ssure filtration.
(1) different modifying agent and consumption are on the impact of property of drilling fluid handled by product
Fig. 2 is the impact of modifier consumption on drilling fluid apparent viscosity, plastic viscosity and yield value.As can be seen from the figure, along with the increase of modifier consumption, apparent viscosity, the plastic viscosity of drilling fluid handled by product reduce gradually, and for the product with the 2-in-1 one-tenth of modifier, after modifier consumption is more than 28%, raising appears again in apparent viscosity and plastic viscosity.And reduce gradually along with the increase of modifier consumption with the yield value of drilling fluid handled by products therefrom, illustrate that the product through modifying can control drilling fluids at high temperature multiviscosisty phenomenon from this point.
Fig. 3 is modifier consumption on drilling fluid handled by product just, the impact of egress.As can be seen from the figure, for modifier 1, along with the increase of modifier consumption, ingressing of products therefrom treated drilling fluid first reduces, after increase again, egress first increases, then reduces, after increase again.For modifier 2, along with the increase of modifier consumption, ingressing of products therefrom treated drilling fluid reduces gradually, and egress first increases, after reduce again.But total trend is the increase along with modifier consumption, first, the egress of drilling fluid reduce.
Fig. 4 is modifier consumption on the impact of drilling fluid API filtration and high temperature and high pre ssure filtration.As can be seen from the figure, for modifier 1, along with the increase of modifier consumption, reduce gradually by the filter loss of products therefrom treated drilling fluid, for modifier 2, along with the increase of modifier consumption, the filter loss of drilling fluid first increases rear reduction.And the high temperature and high pre ssure filtration of drilling fluid significantly reduces along with the increase of modifier consumption, after modifier consumption is more than 23%, slightly rise again, modifier consumption 17% ~ 28% is more favourable to control high temperature and high pre ssure filtration under experimental conditions.
Consider the apparent viscosity of drilling fluid handled by product, plastic viscosity, yield value and just, egress and high temperature and high pre ssure filtration, modifier consumption is better in 23% ~ 28% effect under experimental conditions, and adopts modifier 1 products therefrom performance to be better than modifier 2.
(2) salt dosage is on the impact of property of drilling fluid handled by modified outcome
On the basis of condition experiment, modifier 1 is selected to carry out Product formation (embodiment 1), and (base slurry composition used: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+7% modified outcome+0.5%XJ+0.75%NaOH, increases the weight of to density 2.3g/cm with barite on the impact of modified outcome property of drilling fluid to investigate salt dosage
3), table 1 is the impact of salt dosage on modified outcome rheological, and Fig. 5 is salt dosage on the impact (measuring after 220 DEG C/16h) of drilling fluid filtration handled by modified outcome.
Table 1 salt dosage is on the impact of modified outcome drilling fluid rheology
Note: 1. measure at 55 DEG C; 2. too thickly cannot to measure.
As can be seen from Table 1, in synthesis, introduce the salt resistance that modifier significantly can improve product.From the rheological of drilling fluid, without modifier product (i.e. SMP) handled by drilling fluid anti-salt property poor, and there is high temperature multiviscosisty, and after introducing modifier, obviously can eliminate high temperature multiviscosisty phenomenon, and along with the increase of modifier consumption, the viscosity of residing drilling fluid reduces gradually, and rheological improves further.From high temperature and high pre ssure filtration, along with the increase of modifier consumption, saline-alkaline tolerance improves, and filter loss reduces, but when modifier consumption reach a certain amount of after, then it is little to filtrate reducing influential effect to increase modifier consumption.Under experimental conditions, consider the production cost of product, modifier consumption 23% ~ 28% not only can guarantee system rheological but also can ensure that high temperature and high pre ssure filtration is lower.
3, addition of filtrate reducer is on the impact of property of drilling fluid
Table 2 is dosage impacts on drilling fluid rheology handled by product and filter loss of sample 1 synthesized by embodiment optimization of C/C composites and sample 2.Its drilling fluid forms: the NaCl+0.25% tensio-active agent of 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+0.5%XJ+3.0gNaOH+20%, increases the weight of density 2.3g/cm with barite
3, filter loss is in the aging rear mensuration of 220 DEG C/16h.
Table 2 modified outcome dosage is on the impact of drilling fluid rheology handled by product
Note: 1. measure at 55 DEG C; 2. too thickly cannot to measure.
As can be seen from Fig. 5 and table 2, along with the increase of fluid loss agent sample dosage, filter loss obviously reduces, can the high temperature and high pre ssure filtration of system be controlled within 15ml when dosage is 7%, and drilling fluid rheology improves further after high temperature, illustrate that the thinking of synthesizing high temperature high pressure drop fluid loss agents of the present invention is feasible.
4, Experiment of Compatibility
In order to investigate the adaptability of designed product in drilling fluid further, product of the present invention (representing with HSP) and LP527, MP488, SMC, high-temperature stabiliser etc. are adopted to design the DWSW liquid formula of four groups of different salts contgs:
No. 1: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+7%HTASP+0.5%XJ+0.75%NaOH+0.1% tensio-active agent+10%NaCl, increases the weight of to 2.3g/cm with barite
3;
No. 2: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+7%HTASP+0.5%XJ+0.85%NaOH+0.1% tensio-active agent+20%NaCl, increases the weight of to 2.3g/cm with barite
3;
No. 3: 4% sodium bentonite slurry+1.0%LP527+1.5%MP488+6%SMC+9%HTASP+0.5%XJ+1%NaOH+0.1% tensio-active agent+25%NaCl, increases the weight of to 2.3g/cm with barite
3;
No. 4: 2% sodium bentonite slurry+2.75% stablizer+1.0%LP527+3.5%MP488+6%SMC+6%HTASP+0.5%XJ+1%NaOH+0.1% tensio-active agent+36%NaCl, increases the weight of to 2.1g/cm with barite
3.
According to above four group of formula preparation drilling fluids, and at 220 DEG C aging 16h, measure property of drilling fluid, the results are shown in Table 3.
Table 3 different ingredients property of drilling fluid
As can be seen from Table 3, the drilling fluid of four kinds of different ingredients all has good rheological, high temperature and high pre ssure filtration all≤16ml.Explanation system has good high-temperature stability, and also further illustrating HTASP can effectively control salt-water drilling fluid high temperature and high pre ssure filtration simultaneously.
5, infrared spectra and thermal analyses
(1) from Fig. 6, wave spectrum display is found out, sample 1 has obvious difference with the infrared spectrogram of SMP, and new obvious absorption peaks has appearred in sample 1.Wave number 3403,995cm
-1near have the characteristic absorbance of hydroxyl, wave number 1190,1043cm
-1near have sulfonic characteristic absorbance, near wave number 2931,2875,1444, have the characteristic absorbance of methyl or methylene radical, wave number 3040,1613,1512,1482,833cm
-1near have the characteristic absorbance of aromatic ring, thus prove there are the groups such as hydroxyl, sulfonic group and alkyl in synthesis of product molecules, in synthesis of product molecules of the present invention, comparatively SMP introduces more sulfonic group and oh group.
(2) as can be seen from Figure 7, when temperature rises to 260 DEG C, polymkeric substance starts to decompose, its thermal decomposition process can divide two stages: the first stage occurs between 311 ~ 729 DEG C, corresponding with the thermolysis of methylol, sulfonic group and amido on the base of side, subordinate phase occurs in the temperature section of more than 729 DEG C, and now main polymer chain starts to decompose, visible, product has higher thermostability.
Claims (9)
1. a ultra-high temperature drilling liquid fluid loss agent, is characterized in that: by sulfomethylation resol and formaldehyde, hydroxyalkyl aldehyde, ketone, sulphite, pyrosulfite and water, be obtained by reacting at high temperature under high pressure, wherein each amounts of components is as follows:
2. a kind of ultra-high temperature drilling liquid fluid loss agent according to claim 1, it is characterized in that: described ketone is aliphatic ketone or alicyclic ketone, can be acetone, methylethylketone or pimelinketone.
3. a kind of ultra-high temperature drilling liquid fluid loss agent according to claim 1, is characterized in that: described hydroxyalkyl aldehyde is glycollic aldehyde, 3-HPA, 3-acetaldol, 4-acetaldol, 5-hydrogenation of hydroxypentylaldehyd, 5,5-dihydroxyl valeral or p-Hydroxybenzaldehyde.
4. a kind of ultra-high temperature drilling liquid fluid loss agent according to claim 1, is characterized in that: described sulphite is S-WAT, potassium sulfite or ammonium sulphite; Described pyrosulfite is Sodium Pyrosulfite, potassium pyrosulfite or ammonium pyrosulfite.
5. a ultra-high temperature drilling liquid fluid loss agent preparation method, is characterized in that, comprise the following steps:
(1) massfraction 35% sulfomethylation resol is added autoclave, start stirring, then in reactor, water, formaldehyde, ketone, hydroxyalkyl aldehyde, pyrosulfite, sulphite is added successively by proportioning, raw material adds rear continuation stirring 30 ~ 60min, sealed reactor, heat up, in 70 ~ 90 DEG C, insulation reaction 0.5 ~ 1 hour;
(2) treat that the mixture reaction time of step (1) gained reaches follow-up temperature of continuing rising, at 125 ~ 160 DEG C, react 3 ~ 12h; After reaction times reaches, cooling, pressure release, discharging, through spraying dry powdery product.
6. a kind of ultra-high temperature drilling liquid fluid loss agent preparation method according to claim 5, is characterized in that: the consumption proportion of described sulfomethylation resol and formaldehyde, hydroxyalkyl aldehyde, ketone, sulphite, pyrosulfite and water is:
7. a kind of ultra-high temperature drilling liquid fluid loss agent preparation method according to claim 6, it is characterized in that: described ketone is aliphatic ketone or alicyclic ketone, can be acetone, methylethylketone or pimelinketone.
8. a kind of ultra-high temperature drilling liquid fluid loss agent preparation method according to claim 6, it is characterized in that: described hydroxyalkyl aldehyde is glycollic aldehyde, 3-HPA, 3-acetaldol, 4-acetaldol, 5-hydrogenation of hydroxypentylaldehyd, 5,5-dihydroxyl valeral or p-Hydroxybenzaldehyde.
9. a kind of ultra-high temperature drilling liquid fluid loss agent preparation method according to claim 6, is characterized in that: described sulphite is S-WAT, potassium sulfite or ammonium sulphite; Described pyrosulfite is Sodium Pyrosulfite, potassium pyrosulfite or ammonium pyrosulfite.
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| CN201811355658.9A CN109401736B (en) | 2014-05-30 | 2014-05-30 | Ultra-temperature drilling fluid filtrate reducer |
| CN201410240395.2A CN104293324B (en) | 2014-05-30 | 2014-05-30 | A kind of ultra-high temperature drilling liquid fluid loss additive and preparation method thereof |
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| CN105601853A (en) * | 2015-10-30 | 2016-05-25 | 卫辉市化工有限公司 | Drag reducer for oil well cement, and preparation method thereof |
| CN109401738A (en) * | 2018-12-07 | 2019-03-01 | 中科宝辰(北京)科技有限公司 | A kind of high-temperature-resistant high-salt water-base drilling fluid fluid loss additive and preparation method thereof |
| CN109852353A (en) * | 2019-01-22 | 2019-06-07 | 北京宏勤石油助剂有限公司 | A kind of drilling fluid heat resisting fluid loss reducing agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105601853A (en) * | 2015-10-30 | 2016-05-25 | 卫辉市化工有限公司 | Drag reducer for oil well cement, and preparation method thereof |
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| CN109401738A (en) * | 2018-12-07 | 2019-03-01 | 中科宝辰(北京)科技有限公司 | A kind of high-temperature-resistant high-salt water-base drilling fluid fluid loss additive and preparation method thereof |
| CN109401738B (en) * | 2018-12-07 | 2021-01-01 | 中科宝辰(北京)科技有限公司 | High-temperature-resistant high-salt water-based drilling fluid filtrate reducer and preparation method thereof |
| CN109852353A (en) * | 2019-01-22 | 2019-06-07 | 北京宏勤石油助剂有限公司 | A kind of drilling fluid heat resisting fluid loss reducing agent and preparation method thereof |
| CN109852353B (en) * | 2019-01-22 | 2021-03-16 | 北京宏勤石油助剂有限公司 | High-temperature-resistant fluid loss additive for drilling fluid and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109401736B (en) | 2021-06-01 |
| CN109401736A (en) | 2019-03-01 |
| CN104293324B (en) | 2019-01-01 |
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