Method of forcing liquid through permeable underground formation communicating with well

专利摘要:
A process for displacing a fluid through a well and/or a permeable subsurface formation communicating with the well, by injecting into the well an aqueous solution which contains, as viscosifier, a heteropolysaccharide comprising glucose and, for each 7 moles of glucose, 0.9-1.2 moles of galactose and 0.65 to 1.1 moles of pyruvate, together with succinate and acetate in molar proportions (based on 7 moles of glucose) between 0 and 2. The heteropolysaccharide is suitably obtained by cultivation of a slime-forming species of Pseudomonas, Rhizobium, Alcaligenes or Agrobacterium, in particular Pseudomonas NCIB 11592.
公开号:SU1338785A3
申请号:SU813308250
申请日:1981-05-19
公开日:1987-09-15
发明作者:Эдвард Криппс Роджер；Норман Раффелли Ричард；Джон Стурмэн Энтони
申请人:Шелл Интернэшнл Рисерч Маатсхаппий Б.В. (Фирма)；
IPC主号:

专利说明:

The invention relates to the oil industry, in particular to methods for developing oil fields by pumping water thickened with heteropolysaccharides into a formation.
The purpose of the invention is to increase the efficiency of the process by increasing the viscosity of the solution and maintaining filterability in the presence of ionic salts. Some polysaccharides produced by microorganisms are capable of displacing fluid through wells and / or permeable underground formations connected to these wells. According to the proposed method of displacing fluid through a well and / or permeable underground formation, an aqueous solution containing as an agent that increases viscosity is injected into the well. , heterosaccharide, in which for every 7 mol of glucose is from 0.95 to 1.18 mol of galactose, from 0.70 to 1.08 mol of pyruvate, from 0.85 to 1.25 mol of succinate and from 0.01 to 0.19 mol of acetate.
Heteropolysaccharides of this type are produced by several microorganisms, including microorganisms of the Pseudomonas, Rhizobium, Alcaligenes and Agrobacterium families. In particular, the relevant microorganisms include Rhizobium meliloti, Alcaligenes faccalis bugnyxogenes, Agrobacterium tumefaciens, Agrobacterium radiobacter, Agrobacterium rhizogenes, Pseudomonas of the NCIB 11264 family And, besides, a new strain of the Pseudomonas family of the NIB family 11264 And, in addition, an example of the same type of strain of the Pseudomonas family of the NCIB 11264 family, in addition to the new strain of the Pseudomonas family of the NCIB 11264 family. Industrial Bacteria Collection, Torrey Ricech Station, Aberdeen, numbered 11592.
Heteropolysaccharides, which are used in accordance with the proposed method, are obtained by cultivating the selected microorganism in an aqueous nutrient medium to obtain a sufficient amount. The aqueous nutrient medium contains an assimilable source of carbon and nitrogen along with less significant amounts of magnesium, calcium, iron, phosphorus, and other inorganic ions. Ammonium salt and carbohydrate can be used as sources of nitrogen and carbon, and glucose in concentration can be conveniently used as the latter.
five
0
0.1 to 10 wt.%, Preferably 1 to 2 wt.%. The cultivation temperature and time required to obtain an acceptable yield of heteropolysaccharide depend on the type of organism. When using Pseudomonas of the NCIB No. 11592 family, the temperature is in the range of 20 to 35 ° C. With periodic maintenance, the fermentation time is 60 to 180 hours, preferably 80 to 100 hours.
After fermentation is complete, the heteropolysaccharides can be isolated from the pure fermentation broth or, preferably, the polysaccharides are separated after the cells are separated from the broth by adding the appropriate diluent so that the polysaccharide concentration is about 2000 ppm and then centrifuging the cells from diluted broth. The clarified broth can then be processed in order to isolate the heterosaccharides from the fermentation broth by solvent precipitation, in that the clarified fermentation broth is treated with an appropriate inorganic
0 salt, for example potassium chloride, and a water-miscible solvent which does not react with the heteropolysaccharide and in which the product is insoluble. So the product
g is precipitated and can be isolated using known methods. Then the selected product is dried. Organic solvents that can be used at this stage are
0 linear or branched lower alkanols, e.g. methanol, ethanol and isopropanol, preferably use isopropanol, which is added in a volume that exceeds 1.5 times the volume of clarified fermentation broth.
However, it is not always necessary to separate the pure heteropolysaccharide. The proposed method involves maintaining
g fermentation in equilibrium. In this case, the nutrient medium is continuously loaded into the microorganism reservoir, while the nutrient medium containing the polysaccharide is continuously removed from the system. Then, after the necessary clarification, providing the necessary concentration of it and / or adding other compounds, the medium is injected into the squas: ipu.
five
The heteropolysaccharide that is used in carrying out the proposed method contains octasaccharide blocks based on 7 residues of D-glucose and 1 residue of D-galactose and, in addition, various proportions of some acid residues, namely pyruvate, succinate and acetate. The amount of the components depends on the type of microorganism that is used to obtain the heteropolysaccharide, as well as on the conditions under which the microorganism is cultivated. In addition, in the experimental determination of proportions, some differences are observed between measurements using the same material, which arise partly due to the lack of complete homogeneity of the material and, consequently, due to the presence of differences between samples, and partly due to limitations on accuracy of analytical methods used. Pyruvate is always present in the heteropolysaccharide, and acetate and succinate may be contained in small amounts or absent altogether. As a result of treatment of the polysaccharide with alkali, the succinate and acetate, which were initially contained in it, are completely removed, but the pyruvate content remains unchanged. Such polysaccharides, in which the content of acetate and succinate is zero, possess the necessary physical solutions of ionic salts, which is very important, since aqueous solutions that are used to extract oil are saline, and, moreover, very often formations contain significant concentrations of solk.
logical properties, in particular, the resulting viscosity of the polymer in an aqueous solution, which is necessary to ensure the efficiency of the displacement process. Aqueous solutions of heteropolysaccharides are pseudoplastic or shear thinners, i.e., their viscosity reversibly decreases with increasing cutting speed, so the viscosity criterion depends on the cutting speed. To obtain effective results, the viscosity of a 1000 ppm solution of the heteropolysaccharide in a saline solution of the medium should be at least 3, more preferably at least 10 Mpas, at a cutting speed of 7.5 seconds and 25 ° C. The viscosity under these conditions is determined using Brookfield LVT or Contrave's Low Shear viscometer, or Dir rheometer.
Agents that increase the viscosity of aqueous solutions, in turn, are used as agents to displace fluids (such as petroleum
in underground permeable formations in the active well (or several active wells). The oil is then removed to the surface through the active well (s). In accordance with the proposed method of increasing oil recovery using water pressure, water viscous
solutions have a significantly higher injecting capacity compared to a fluid that has similar displacement characteristics, but has Newtonian flow properties. However, the forcing is
the property can be significantly reduced by holding the polymer in the pores of the permeable underground formation, which leads to clogging
then with the subsequent decrease in the forcing ability and decrease in extraction of oil.
To analyze the potential hazards of driving an education that has
a certain permeability, carried out the appropriate tests associated with filtration. At the same time, a polysaccharide obtained by cultivating
microorganisms, in accordance with the proposed method. It was found that such a danger is minimal. The filterability characteristics of the polysaccharide solution are maintained at
but, since the aqueous solutions that are used to extract the oil are hydrochloric, and, in addition, very often the oil-bearing formations themselves contain significant concentrations of solc.
The characteristic properties of the Pseudomonas culture of the NCIB 11592 family. The morphological and physiological characteristics of this culture: microorganisms possess many characteristics of the Pseudomonas species, as well as some properties that are characteristic of Agrobacterium, however, under some conditions, water-soluble pigment is produced, they belong to the Pseudoonas family .
Physical characteristics.
Small sticks, found ak separately, and in pairs, 0.5-1.0 x1.5-2.5 microns. Movable with 1 or 2 polar antennae. There are no obvious signs of spore formation (or cysts). Gram staining is negative.
Some characteristics of growing neither.
Nutrient agar plate. The colonies are not quite white, flat with even gloss, round shape and solid. Diameter 2-3 mm after 24 hours at.
Physiological characteristics.
Catalase - positive; oxidase - positive; carbamidase is positive.
Growth aerobic and anaerobic with nitrate.
Relation to temperature - up to 37 ° С is optimal at 30 ° С. Growth is absent at 4 or 41 C.
The relation to pH is optimal 6.5–7.5, the limit is 4.5–9.0.
Methyl red - negative
Vodzhes-Proskauer - negative.
The destruction of hydrocarbons is oxidative.
Output is negative.
Indole production is negative.
The reduction of nitrate is positive, with the formation of N or NHj.
Hydrolysis: gelatin - negative; tvina - negative; casein - negative; starch - negative.
Litmus milk - restorative. Arginine dihydrolase (Thornle test) - negative; arginine decarboxylase - negative; lysine decarboxylase - negative ortin decarboxylase - negative
Pigmentation - Kings B medium, slightly yellow color.
The use of carbon sources on glucose, sucrose, fructose, succinate, serine, alanine, mannitol, lactate and propylene glycol, on acid derived from glucose. No growth is observed on citrate, malonate, phenylalanine, gluconate, ethanol or ethylene glycol.
The test of Bernaerts and De Le is positive.
I
Production of heteropolysaccharides by cultivating the microorganism Pseudomonas of the NCIB 11592 family.
Batch process.
Batch cultivating material is produced by growing one colo
338785
The Pseudomonas Seme / Yutr NC1K 11592 on an agar plate in a 250 ml conical flask, which is shaken periodically.
five
0
five
This papillary contains Lebmko's broth (l00 ml) and 10 g / l of glucose, the cultivation is carried out at 30 ° C for 24 hours on an orbital shaker. A portion (40 ml) of this culture is then transferred under sterile conditions to a conical shake flask containing 1 l of medium, the composition of which is described below. Further, the incubation is carried out for an additional 30 hours at 30 ° C on an orbital shaker before the grafting material is placed in the fermenter.
g / l:
0
The composition of the medium. Glucose Na, HP04 KHjP04
Hjboj
Nail .oOt 2НГО
10 3.0 3.0 0.3 0.2 The medium contains,
66,8
14.7 0.36 0.32 0.30 0.36 0.20 0.60
Fermentation is initiated by the addition of a graft material to a Shemap LF-7 type fermenter containing 3 liters of growing medium, up to 4 liters. The culture temperature is maintained at the level of 2810.2 C, and the pH is at the level of 6.80, by adding 1 n. potassium hydroxide solution + 1 n. sodium hydroxide solution. Air is bubbled into the fermenter at a rate of 0.50 l / min and the culture is stirred using 3 Rushton-type turbine mixers equipped with 4 paddles at a speed of 1000 rpm. Gas transfer under these conditions is sufficient to maintain the elasticity of oxygen dissolved in the culture in the range of 120 to 140 mm Hg.
Regularly during fermentation, samples of culture broth are taken.
(20 ml) and analysis of cell and exopolysaccharide concentrations, residual glucose in the medium and residual ammonium ions in the medium is carried out.
After the fermentation is complete, the broth is separated from the cells, diluted with water to a polysaccharide concentration of 2000 ppm in the broth. Then the broth is thrown back to centrifugation using Sharples laboratory supercentrifuge at a feed rate of 3 l / h. Then, the heteropolysaccharide is removed from the fermentation broth by adding potassium chloride and then isopropanol in an amount that exceeds the volume of the clarified fermentation broth by 1.5 times. The resulting gel-like precipitate is removed from the depleted fermentation broth, and then pressed to remove residual isopropanol and dried under vacuum at. The dried material can then be converted into a finely divided powder.
The process of continuous action.
The Pseudomonas NCIB 11592 culture broth is placed in a 4-liter Biotech enzyme equipped with valves and a turbine to mix the NIN. Then two nutrient streams are fed to the broth: 1 g / l stream: 1.088; MgSO. 0.493; 0.147; glucose 20, other elements of the medium as described above; stream 2: (21.14 g / l.
The volume of the broth is 2.6 L, the feed streams 1 and 2 function continuously at a speed of 149.2 and 15.4 ml / h, respectively. The temperature of the culture broth is maintained at 28 ° C, the pH is 7.5 using 2.0 n. a solution of a mixture of sodium hydroxide and potassium hydroxide. The culture medium is continuously removed from the fermenter at the same rate, with the output stream containing 3.7 g / l of polysaccharide (viscosity estimate) and 2.7 g / l of cells in dry form (optical density estimate).
Determination of the chemical structure of the heteropolysaccharide.
The heteropolysaccharide obtained according to the batch fermentation process is hydrolyzed using a 0.25 M solution of sulfuric acid at 95 ° C for 16 hours.
Quantitative analysis using GLC after conversion to peracetylated aldononitrile derivatives, as well as using enzymatic methods, showed that neutral sugars are only in the form of D-glucoea and D-galactose; the molar ratio of glucose to galactose is 7: 0.96; for every 7 moles of glucose, respectively, 1.02; O, 11 and 1.11 mole
As a result of the titration of the deionized natural polysaccharide, the curve for the expected diacid acid was obtained, while the titration of the deacylated alkali polymer indicated one acid group.
Consequently, the polysaccharide contains an alkali-stable acid group, which is provided with a priruvate group, linked as ketal to the sugar residue, and, moreover, an acid group unstable with respect to alkali, which is formed from succinic acid, in the form of its partial ester. The content of acetyl in the polymer varies from one batch process to another, however it is always less than the molar content of galactose. Succinid content is approximately equal to the molar content of galactose.
As a result of the methylation of the polysaccharide using the Hakomori procedure, methylated sugars are obtained, which are listed in Table 1. Complete sugar analysis is obtained using two GLC systems. Individual methylated sugars are identified by GC-MS.
The presence of two different 2,4,6-tri-0-methyl derivatives of hexose showed that galactose and glucose residues are connected in 3 positions of the molecule. The remaining partially methylated sugars are derived from glucose residues.
Methylation data is best interpreted using polymers with 8 sugar units (7 glucose + 1 galactose).
No evidence of tetramethyl derivative was found, but there were two blocks of 2,3-di-O-methyl glucose per link.
Therefore, if this link is branched, the non-reducing end should consist of 4.6, O- (1-carboxyethylidene) -B-glucose, pyruviated glucose residue, which gives 2,3-di-0-methyl glucose during methylation. The second residue of 2,3-di-O-methyl glucose must be obtained from sugar at the branch point of the polysaccharide.
To estimate the size of the polysaccharide composition for a particular microorganism strain, several polysaccharide samples were prepared from a Pseudomonas NCIB 11592 family culture, and then the product was subjected to enzymatic analysis after hydrolysis in a 0.25 M sulfuric acid solution for 16 hours. The results are shown in Table 2. .
A detailed study was carried out on 6 products obtained by periodically conducting a fermentation process using Pseudomonas of the NCIB 11592 family. Sugar and acid tests were carried out using high-pressure liquid chromatography using a Bio-Red HPX 87 column with a height of 30 cm at 30 ° C in order to detect UV absorption in the region of 206 nm. The number of samples that were analyzed was from 3 to 5 for each batch mode, with each sample being hydrolyzed separately. Differences between samples of each batch process were statistically processed to obtain a standard error of the mean for each batch mode. When determining the content of galactose by an analytical method, the standard deviation was 0.05.
The results are shown in table 3.
In all cases, ace tat was detected, but its content was so small that exact figures were difficult to obtain (molar ratio of about 0.3).
Sugar analyzes were carried out for polysaccharides produced by several known organisms. The results are summarized in table 4.
From the results shown in Table 4, it can be seen that the polysaccharides produced by each organism (including the new Pseudomonas of the NCIB 11592 family) have the same content of sugar and pyruvate; accordingly, they all have the same basic octasaccharide unit, which has been fully studied in connection with the polymer obtained using the Rhizobium meliloti strain; all polysaccharides having such a composition are potentially
suitable for use in the proposed method.
Determination of the rheological properties of heteropolysaccharide.
Viscosity and shear rate were determined for polysaccharides prepared using several microorganisms. The results obtained are summarized in table.5. In all cases, the results refer to a solution of 1000 ppm polysaccharide in a saline solution of the medium; measurements were carried out as described.
The effect of salinity on viscosity was also evaluated using a polysaccharide from the Pseudomonas culture of the NCIB 11592 family in a 1000 ppm aqueous solution containing various concentrations of sodium chloride. All measurements were carried out at 25 ° C and the shear rate.
The results are shown in table 6.
Phptability
The potential likelihood of blocking was evaluated by empirical filtration testing, according to which the transit time of a given volume of heteropolysaccharide solution through a certain filter (s) was measured.
The solutions were easily filtered for a long time, if
at least part of the filter is open to the flow, but as soon as the filter pores clogged, the filtration rate dropped sharply. Empirically found that the filtering process can be
satisfactorily evaluated using filters with a diameter of 47 mm with a pressure drop of 1.0 bar and a sample volume of 100 ml of solution. Suitable for these purposes are cellulose ester type filters (for example, Millipore), having a pore size of 0.45 to 5 microns, for example, 0.45; 0.8; 1.2 or 5.0 microns. The corresponding characteristic is expressed as the time required for 100 ml to pass through the filter. To determine the effect of ionic salts on the filterability characteristics, a filtration test was carried out for three salinity levels, namely:
low salt content - 0.5% NaCl AND 0.05% CaClj 2FjO; the average salt content is 3% NaCl and 0.3% CaClj; high salt content is 10% NaCl and 1% 2HiO.
The brine is prepared with a heteropolysaccharide concentration of 600 ppm, then the filterability is evaluated as described above. In determining the filtration characteristics of a heteropolysaccharide produced by the Pseudomonas culture of the NCIB 11592 family, it was established that at all levels of salinity, the solutions passed through filters with a pore size of 0.8; 1.2 and 5.0 microns in less than 3 min. In all cases, it was found that the passage of the solutions through the filters did not lead to any reduction in the resulting viscosity of the polymer solution. When using the filter with the smallest size
0.45 µm filtering time is determined by the earth formation in the direction of
whether for polysaccharides produced using several microorganisms.
The test results are summarized in Table 7.
For the Pseudomonas culture of the NCIB 11592 families, 600 ppm polymer solution was tested and used; for polymers prepared using other organisms, a solution of 1000 ppm was used.
Stability cut.
The assessment of the stability of the slice of the polymer obtained using the culture of Pseudomonas family NCIB 11592, produced as follows
A 400 ml container was placed in a Sorwell Omnimixer device, ice-water cooled by a mixture. Approximately 175 ml of polymer solution with a concentration of 1000 ppm and a mixer were turned on at 11,500 rpm. The initial sample was taken, after 30 seconds, 1 minute, 2 minutes, 4 minutes, 8 minutes and 16 minutes, which gave a total cutoff time of 30 seconds. for 1 min, 2 min, 4 min, 8 min and 16 min, respectively. Samples were taken (4 ml) with a Pasteur pipette and the viscosity (mPa-s) was determined at a cutting speed of 23. The results were compared with the results obtained for known viscosity agents used in oil production: Kelzan XC and Pushner 700. The viscosity of the first and last samples from the Kelzan experiment was measured after 1 day of measurement showed the absence of any measurable viscosity recovery.

table.8.
The high resistance to salt and slice, as well as the low blocking ability, allow the proposed polysaccharide, obtained with the help of microorganisms, to be used as a viscosity agent in processes in which aqueous solutions are used to displace fluids in wells and / or subterranean formations. x connected to the well. With
use as an agent of viscosity in a process whereby a viscous aqueous solution of extrusion is used to displace oil or other hydrocarbon mixtures into
B
the current well (or operating wells), the higher viscosity of the fluid displacement effectively minimizes the formation of fluid lines in the body of oil contained in the formation. The resistance to shear and resistance to the effects of the salt of the proposed polysaccharide ensures the preservation of the necessary physical properties of the fluid until it again appears on the surface together with the extracted oil.
The proposed method can be used not only to displace oil, etc. in the oil fields in the direction of the existing well, but also to clean the well by displacing the liquid that was originally contained in the well. This procedure is in this case part of the repair work or the final preparation of the well. The cleaning of the well is necessary after the casing has been cemented and 5 before the start of oil production. For these purposes, viscous saline and heteropolysaccharides are used, which are highly effective as Q viscosity agents, since they are highly resistant to salt and do not form clogging. Salt resistance allows the use of hydrochloric acid as a cleaning fluid, since it has a higher density than water. In addition, the formation of blockings in oil reservoirs is unlikely when part of the viscous
The liquid solution enters the pore space of the reservoir at the level of the connection between the reservoir and the well.
To clean the well, a viscous saline is injected into the well through a pipeline located in the well. The solution then returns to the surface through a gap around the pipeline. The fluid that was originally contained in the well is displaced by a circulating viscous saline solution, while at the same time solid particles in the well are lifted to the ground. Solids are removed from the circulating viscous saline as a result of the saline passing through the filter on the top. The proposed method can be used for well repairs. In this case, the well is cleaned, displacing the fluid contained in it. The fluid to displace remains in the well while repair operations are being carried out. To prevent the release of the well, the cleaning fluid can be loaded onto 10 with the help of appropriate loading agents to increase the density of the fluids used to treat the wells.
1-15

权利要求:
Claims (1)
[1]
Invention Formula
A method for displacing fluid through a permeable subterranean formation associated with a well by injecting an aquatic plant through the well. Since a viscous saline solution thickened with a viscosity agent, a thief has a low ability to
In filtering, cleaning the filter is essential to increase the efficiency of the process only when the amount of solid is increased by increasing the viscosity of the dissolved particles so that the filterability in Prioni is reduced by the filtration rate. In the presence of ionic salts, in the reservoir of the reservoir of the cleaning of the well, a viscous salt-resistant water solution containing
As a viscosity agent, a heteropolyaccharide obtained by cultivating a Pseudomonas culture, the solution temporarily remains in the well until the final work on its preparation in the well. In addition to use in wells for the production of NCIB 11592, which contains
Oil, the proposed method can also be applied at the final stages of well preparation, including the injection of fluid into the reservoir for oil propellants.
The proposed method can be used in the repair of wells. In this case, the well is cleaned, displacing the fluid contained in it. The fluid for displacement remains in the well, while repair operations are carried out in it. To prevent release from the well, the cleaning fluid can be loaded with suitable loading agents to increase the density of the fluids used to treat the wells.
1-15
glucose and for every 7 mol of glucose from 0.95 to 1.18 mol of galactose, from 0.70 to 1.08 mol of pyruvate, from 6.87 to 1.25 mol of succinate and from 0.01 to 0.19 mol of acetate .
Table 1
2,4,6-Glucose 2,4,6-Galactose 2,3,6-Glucose I
2.06
1.00 2.91
Note. Column 1 5% SE 30 on suploco port 100/120; 175 C; N3 at a rate of 50 ml / min. Neopentyl glycol adipate column on the W.A.W chromosorb; N at a rate of 50 ml / min; 2,4,6-glucose is 2,4,6-tri-O-methyl glucose.
with a periodic process
in a continuous process
Table 3
Microorganism
Pseudononas sp NCIB 11264
RhizDbiun meliloti
Rhizobiun neliloti DSM 30136
Agrobacterium radiobacter
NCIB 8U9
Agrobaclegium radiobacter
NCIB 9042
Agrnbarteriun tumfaciens
DSM vr DK
1338785
16 Table 2
Table 4
Sugar, "or
Acid ociaTKH, Gel
Glucose Gpaktoea Pyruvlt Acetate Sukiina
0,940,910.090,67
1,001,001,201,65
1,051,021,071,98
1.05
0.98 0.350.74
0.941.00 0.140.57
0.970.89 0.160.51
Pseudonranas sp. NCIB 11592
Paeudomonas sp. NCIB 11264
Rhizobium meliloti K24
Agrobacterium radiobacter
NCIB 8149
Deacylated NCIB 11592 culture product
Pseudomonas family
NCIB 11592
Pseudomonas family
NCIB 11264
Rhizobium meliloti K-24
Agrobacterium radiobacter
NCIB 8149
2212
2112
149.0
129.0
1210.4
Table 7
360
260 208
108
Editor L.Pcholinsk
Compiled by I. Lopakova
Tehred I.PopovichKorrektor A.Obruchar
Order 4151/59 Circulation 532 Subscription
VNIIPI USSR State Committee
for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
Production and printing company, Uzhgorod, st. Project, 4

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GB8622032D0|1986-09-12|1986-10-22|Shell Int Research|Aqueous polysaccharide compositions|

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FR2634219B1|1988-07-13|1992-04-24|Rhone Poulenc Chimie|NOVEL HETEROPOLYSACCHARIDE BM07, METHOD FOR PROVIDING IT AND APPLYING IT IN VARIOUS TYPES OF INDUSTRIES|

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FR2652820B1|1989-10-09|1993-12-24|Rhone Poulenc Chimie|STABLE SUSPENSIONS OF ZEOLITES COMPRISING A SUCCINOGLYCANE.|

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US5184679A|1991-11-27|1993-02-09|Shell Oil Company|Gravel packing process|

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US5251699A|1992-05-26|1993-10-12|Shell Oil Company|Low-viscosity gravel packing process|

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US5881826A|1997-02-13|1999-03-16|Actisystems, Inc.|Aphron-containing well drilling and servicing fluids|

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FR2784395B1|1998-10-13|2002-12-27|Rhodia Chimie Sa|HETEROPOLYSACCHARIDE PRODUCED BY AN AGROBACTERIUM RADIOBACTER|

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US6746992B2|2001-07-25|2004-06-08|M-I, L.L.C.|High density thermally stable well fluids|

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US8287210B2|2010-11-17|2012-10-16|Amcol International Corporation|Sub-aqueous placement of water-based suspensions and method of manufacture and use|

法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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GB8016832|1980-05-21|

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