|Publication number||US3291214 A|
|Publication date||Dec 13, 1966|
|Filing date||Aug 19, 1964|
|Priority date||Aug 19, 1964|
|Publication number||US 3291214 A, US 3291214A, US-A-3291214, US3291214 A, US3291214A|
|Inventors||Hower Wayne F|
|Original Assignee||Halliburton Co|
|Export Citation||BiBTeX, EndNote, RefMan|
|Patent Citations (5), Referenced by (7), Classifications (7)|
|External Links: USPTO, USPTO Assignment, Espacenet|
United States Patent 3,291,214 DISPERSION METHOD OF SAND CONSOLIDATION Wayne F. Hower, Duncan, Okla, assignor t0 Halliburton Company, Duncan, Okla., a corporation of Delaware No Drawing. Filed Aug. 19, 1964, Ser. No. 390,730 20 Claims. (Cl. 166-33) This application is a 'continuation-in-part of US. application Serial No. 130,763, filed August 11, 1961, now abandoned, and is entitled to the benefits of said earlier filing date as to all common subject matter.
The present invention relates to a method of consolidating loose sand in hydrocarbon bearing formations and more particularly to a new and improved method wherein consolidating resins, silicates and other consolidating materials are dispersed in a low viscosity non-miscible fluid and then introduced into the formation to be consolidated.
Prior art methods of applying consolidating resins, silicates and other consolidating materials to hydrocarbon or oil bearing formations have been by the slug method. In the slug method, a quantity of consolidating material, such as sodium silicate, a phenolic resin, epoxy resin, and other suitable resins or the like, is forced into the sanding formation and then overdisplaced with oil' Such a method using sodium silicate as the con solidating material is described in copending application U.S. Serial No. 29,174, filed May 16, 1960, and now abandoned. The overdisplacement of the oil assures that all of the consolidating material is out of the tubing and casing, develops permeability in the saturated sand, and in some applications hastens the hardening or setting of the consolidating material when a hardening agent has been included in the displacing oil.
This system although being very effective in many instances has certain disadvantages. If the displacing oil or fluid is used in excessive amounts, the oil or fluid has a tendency to partially or, in some instances, completely remove all of the consolidating material from the sand grains. This results in a very poor consolidation, it any, adjacent to the perforation, and consequently an unsuccessful sand consolidation attempt. As it is difficult to keep track of small volumes of consolidating materials, the minimum quantities used often exceed the amounts actually needed. The cost of the consolidating materials is therefore greater than necessary. It is therefore an important object of the present invention to provide a new and improved sand consolidation method which overcomes these disadvantages.
The present invention, which is sometimes referred to hereinafter as the dispersion method of placement, is an improvement over the slug method of placement or other prior art methods and has several additional advantages over such methods which have been substantiated by laboratory and field tests. Some of these advantages are: The compressive strength of consolidations adjacent to the perforations is better (good consolidation is essential at this point for successful sand control), a lower viscosity consolidating material can be used, which is more desirable for consolidation applications; consolidation is more evenly distributed throughout the treated sand; and compressive strength and retained permeabilities are more constant.
An important object of the present invention is to provide a new and improved method of consolidating sands in oil bearing formations wherein the consolidation resulting from the use thereof is of a high compressive strength adjacent the perforations and is evenly distributed throughout the treatedsand.
Another object of the present invention is to provide a new and improved method of consolidating sands in oil bearing formations wherein a low viscosity consolidatice ing solution is used thereby facilitating injection of the consolidating soluton into the formation to be treated.
Still another object of the present invention is to provide a new and improved method of consolidating sands in oil bearing formations, which is not only more economical than prior art methods, but which also may be performed more readily and easily than prior art methods.
Other objects and advantages of the present invention will be more readily apparent from a reading of the specification hereinafter.
Broadly, the dispersion method of placement comprises dispersing a consolidating solution such as a liquid resin, sodium silicate or other suitable consolidating solution in a low viscosity non-miscible fluid, such as diesel oil or the like, and then pumping the fluid into the formation to be treated.
The viscosity of the non-miscible fluid should not exceed about ten centipoise at a normal room temperature and pressure, and in the preferred form of the invention, the viscosity of the non-miscible fluid should not be more than about five centipoise. The viscosity of diesel oils varies from about two to about ten centipoise at normal room temperature and pressure, with most oils having a viscosity about three centipoise. Normal room temperature for laboratory experiments was 77 F. and pressure was standard atmospheric pressure of 14.7 psi.
The preferred ratio of consolidating material to oil or carrying fluid is from about 1 to 1 up to about 1 to 4, and it is generally preferred that the volume of oil exceed that of the consolidating solution.
It should be noted that although the ratio of consolidating material to the oil carrying fluid is preferably less than 1 to 4, greater ratios may be used satisfactorily, depending upon the viscosities and nature of the liquids involved.
In the most desired dispersion, small drops of consolidating material and oil alternate in entering the sand body. This results in a continuous placement and displacement of the consolidating material into the formation, and the probability of mechanically washing all of the consolidating material from the sand grains is practically nil.
It should be noted that the dispersion as set forth in this invention is not an emulsion. The consolidating solution substantially settles out of the oil in 30-45 seconds. Most emulsions would not enter the permeability of a sand formation and are therefore undesirable. The selection of the chemical which forms the consolidating material-oil dispersion is very important. Some chemicals, although forming a good dispersion, will have a tendency to cause the consolidating material to enter the sand slowly and filter out on top of the sand and let the oil by-pass into the sand.
The present invention or dispersion method of sand consolidation consists basically of preparing a physical mixture of low viscosity oil and consolidating solution, adding a dispersing agent thereto when needed, adding a setting or curing agent to the solution either prior to plac ing the mixture in the formation or afterwards, depending upon the type of consolidating solution used, and pumping or otherwise introducing the mix-ture into the desired formation.
Various consolidating solutions may be used without departing from the present invention. Successful laboratory and field tests have been made using sodium silicate, and thermosetting resins such as phenolic and phenolicresorcinol formaldehyde resins and various epoxy resins.
Other resins such as polyesters, urea-formaldehyde or any other suitable consolidating material capable of being dispersed may be used without departing from the scope of the invention. To these consolidating solutions is preferably added a dispersing agent. Dispersing agents successfully tested include, Hyfio and a mixture of Hyflo with a substituted imidazolene for sodium silicate; sorbitol sesqui tall oil for the phenolic resins and diethylaminopropylamine and dimethylaminomethyl phenol for epoxy resins. In the case of the latter, the dispersing agent is actually the catalyst for the epoxy resin and no special or additional dispersing agent is necessary.
Although some dispersion may be obtained by agitation of the consolidating solutions with the oil, a suitable dispersing agent aids considerably in dispersing the consolidating solution in the oil, and further aids in the displacement of the consolidating solution into the formation.
The above referred to dispersing agents may be identified more specifically as follows:
Hyflo.The trade name of a surfactant or surface active agent sold by Halliburton Company. It is a mixture of anionic and nonionic surfactants manufactured by Visco Products Company and described in US. Letters Patent No. 2,946,747.
Substituted imidazolene.A cationic oil soluble surfactant which is 15% isopropyl alcohol with the active ingredients being chiefly a substituted imidazolene.
Sorbitol sesqui-tall oil.A nonionic oil soluble surfactant or surface active agent, marketed by Atlas Powder Co., Aquaness Division under the designation PR-383.
Although the dispersing agent or surfactant may be added to the dispersion fluid at any time prior to introduction into the earth formation, it would normally be added to the oil or non-miscible fluid prior to the oil and consolidating material being mixed together to form the dispersion fluid.
As the quality of crude oil varies greatly from one formation or pool to another, it is usually necessary and highly desirable that the sand of the crude oil be cleaned or flushed out. This is normally the first step in any sand consolidation method and is recommended with the dispersion method of the present invention. Any suitable oil or sand cleaning agent may be used in this step, and such step has been successfully performed using a mixture of diesel oil and Hyflo. The cleaning agent washes or cleans the sand grains in the treated formation thereby enabling a good contact of the consolidating material with the sand grains.
In the present invention, the specific method steps as well as the specific chemicals or materials used in each step varies with the type of, or particular consolidating material selected for-the overall sand consolidation operation. An example of the present invention wherein sodium silicate is used as the consolidating material is as follows:
EXAMPLE I (1) A diesel oil-Hyflo mixture is pumped into the formation for cleaning the sand grains. This step may be preceded by a pre-flush step, if desired, using a mud cleanout agent or other suitable agent.
(2) Sodium silicate and a dispersing agent are dispersed in diesel oil or other suitable carrying fluid. A 30% sodium-silicate dilution may be used Whereas in the slug method, the dilution of sodium silicate is normally not more than The dispersion is a physical mixture of preferably about 1% to 2 volumes of oil to one volume of sodium silicate. Even though the dispersion may be relatively stable, some agitation is preferred. A ribbon blender of 25-30 barrels capacity has been used satisfactorily, and air agitation is also quite effective in maintaining the dispersion, once the dispersion has been obtained.
(3) The mixture or solution is then introduced into the well, normally by way of the tubing. The turbulent flow of the fluid is sufficient to keep the consolidating solution suspended therein. A pump rate of /2 to 1 barrel per minute is recommended. Pumping should not be stopped while the dispersion is in the tubing as pronounced separation may occur.
(4) A setting agent such as 20% cresol in oil solution is pumped into the formation to set the sodium silicate.
(5) An additional stabilizing solution such as a 20% calcium chloride duohydrate solution may be pumped into the formation to further stabilize the set of the sodium silicate and give it additional strength.
Some examples of tests made using sodium silicate of various viscosities (or dilution) are set forth hereinbelow. Each test was performed at F. using glass tubing of inches internal diameter and Oklahoma #1 sand. The diesel oil preflush of step 1 contained 1% fHyflo. Fresh water was used as the diluent.
Test I.Using sodium silicate as received from normal commercial sources. Viscosity, 50 cp.
Compressive strengths good, permeability retention was unsatisfactory.
Test II.--Using sodium silicate diluted 10% Viscosity, 25 cp.
E F G Diesel Oil, cc .1 4O 4O 40 Hyflo, cc .4 .24 Substituted imidazolene, cc 15 .18 Sodium Silicate, cc 20 20 20 Compressive Strength, p. 1,130 1, 710 1, 300 Permeability, md 4, 330 3, 608 738 Test III.Using sodium silicate diluted 20%. Viscosity, 17 cp.
Diesel Oil, cc 40 40 40 Hyflo, cc 14 24 Substituted imidazolene, cc 18 18 Sodium Silicate, cc 20 20 20 Compressive Strength, p.s.i 852 1, 420 1, 050 Permeability, Ind 3, 910 3, 521 4, 470
Test lV.Using sodium silicate diluted 30%. Viscosity, 14 cp.
K L M Diesel Oil, cc 30 30 30 Hyflo, cc .3 18 Substituted imidazolene, cc 135 Sodium Silicate, cc a. 20 20 2O Compressive Strength, p.s.i 850 1,110 925 Permeability, md 5, 323 5, 036 5, 548 2 stage testPermeability, md 4, 218
Using various resins, some comparative tests were made using the slug method and the dispersion method. Some examples of these tests and the results therefrom are as follows:
Test A The basic formula used to prepare the resin was:
33.2 grams of (a phenolic resin) 25 grams of (a resorcinol resin) 25 cc. isopropanol 5 cc. 10% sodium hydroxide solution A laboratory consolidation made with this formula and flushed with 2'volumes of oil gave a compressive strength of 148 p.s.i. Another consolidation using 1 volume of resin and 4 volumes of diesel oil containing 1% sorbitol sesqui-tall oil as the dispersant gave a compressive strength of p.s.i. Similar tests made in a large cham- 6 In the two stage treatment the sand is treated with the dispersion twice.
Field test Slug Method Disperslng en nacua e es wasmaeinawe in e 100): Mtd A t lfildt t d 11 th W1 sand, Clearbrook Field, Cleveland County, Oklahoma, as Side of perforation md 1 0 751 fOllOWSC Below the perforatmmd 298 m The well treated was completed quite some time previousl as a flowin well. A um was installed later These data illustrate how the dispersion method gives when Wen Startid to make i with fluid Produc nfiore avert peFmeablhtles' The appearance of tion being 500 b.p.d. (barrels per days) (5% oil) just prior Li i 5 f zg dmdlcated a much to the sand consolidating job. The well would make 6 er S lane or e lsperslon me O sand, but it would not sand up until pumping was stopped. I Test B Two cleanouts were performed before a produced sand The following basic formula was used for this test sample could be obtained. when treating the 3.5 cubic feet of sand in the large It Was decided to use two 2-drum stages of the disperchamber: sion in perforations from 7118 to 7122 feet. Tubing ca- Formaldeh de cc 2800 pacity for the 2-inch tubing was 40 barrels. An RTTS pores 01 560 packer was used in the placement with salt water being in Guanidine carbonate r n igggg mien was re aredasfonows. 50% sodium hydroxide solution cc 125 p p (1) Two drums (110 gallons) sodium silicate lus The above chemicals gave one gallon of resln. gallons fresh water p I In tl'fie sl3u; treatmlenhhe rlesin1 wals ilisplacied gkithd5 g 2 (2) 5.1 barrels diesel oil containing 1 gallon substituted ons o a 0 creso 1n iese o1 souion. n e ispero imidazolene and 15 anOnsH fio sion treatment, the one gallon of resin was dispersed in g y 4 gallons of diesel oil containing 1% sorbitol sesqui-tall The two solutions were mixed by circulating in the oil as the dispersant and 1.2% cresol. The following retank to glve a good d1spersion. This dispersion would sults were obtained when the consolidations were prepared settle out slowly in time but it was kept suspended very at 120 F. 30 easily by bubbling a small stream of air through the fluids.
Slug Method Dispersion Method Strengths, Permeabilities, Strengths, Permeabilities,
p.s.i. md. p.s.i. md.
Below Perforation .1 60 5,390 320 6, 605 Side of Perforation 320 4, 547 420 3, 424 Bottom of Consolidation 140 3, 727 380 3, 551
Additional observations indicated a more consistent strength for the dispersion treatment right at the perforation and the outer extremities of the consolidation.
Test C Using an epoxy resin and diacetone alcohol as the solvent therefor.
Epon 820 was diluted with an equal volume of diacetone alcohol to give a resin solution having a viscosity of 28 cp. at 77 F. For the slug method, the sand was treated with one volume of resin containing 0.8% diethylaminopropylamine as the catalyst and then flushed with 2 volumes of diesel oil containing 0.8% of the same catalyst. The top of the sand was not consolidated as the oil had removed all of the resin. The bottom 50% of the treated sand had a very poor and weak set. No permeabilities or compressive strengths could be determined. A dispersion was made using 1 volume of resin and 2 volumes of diesel oil containing 0.8% diethylaminopropylamine (based on the total volume of resin and oil). No additional chemical was used to form the dispersion as the catalyst was an effective dispersing agent. The consolidation had a compressive strength of 835 p.s.i. and a retained permeability of 5328 Ind.
Epon 820 is a well known epoxy resin marketed by Shell Chemical Co.
The dispersion method of the present invention may be performed in what is referred to as a one stage system or a two stage system. The one stage system is the carrying out of an operation whereby the sand formation to be consolidated is treated one time with the dispersion.
LOG OF TREATMENT Pump pressure Fluids used when fluids Pump rate, were placed bbL/minute in tubing, p.s.i.
l0 bbls. diesel 0il+5 gals. Hyfio 1,400 1% 8.5 bbls. of dispersion 1,800 1% 5 bbls. setting solutioi1+2% gals. Hyflo. 1, 500 1% 14.5 bbls. stabilizing solution normal concentration) 1, 500 to 1,700 1% 10 bbls. salt water 1, 500 to 1, 400 1% 30 bbls. crude oil 1, 300 to 1,200 10 bbls. diesel oil+5 gal Hyfi 1, 350 to 1,700 1% 8.5 bbls. dispersion l, 900 1% 5 bbls. setting solution-lgals.
Hyflo 1, 900 1% 15 bbls. stabilizing solution 1, 900 to 1,700 1% 40 bbls. salt water 1, 500 to 1, 000 1 Total time for job-2 hours and 40 minutes.
Well closed in at finish. Tubing pressure dropped to 400 p.s.i. in 2 minutes, 200 p.s.i. in- 4 minutes and p.s.i. in 7 minutes.
All solutions were mixed before bringing them to the location. The job was handled with one acid truck and two tank trucks and the entire job went off very well mechanically.
The change in pump rate from 1% to %1 barrel per minute was made to introduce the dispersion to the formation at a 2 gallon per minute per perforation rate.
The exact pressure on the formation when the dispersion entered the formation would be fairly difficult to calculate due to the many different fluids being in the tubing 7 at the same time. It is believed that a 150 to 250 p.s.i. increase in pressure was noted for the entrance of both stages of the dispersion and the overall pressure for the second stage was a little higher than for the first stage.
Two weeks after the treatment, the well was producing its normal 500 barrels of fluid a day with no sand.
The problems of sand consolidation and the importance of using a low viscosity consolidating solution are discussed at length in an article by the inventor, entitled Large-Scale Laboratory Investigation of Sand Consolidation Technique, published in the December 1961 issue of Journal of Petroleum Technology.
The present invention makes possible the use of the desired low viscosity consolidating solution.
Broadly the present invention relates to the introduction or injection of a solution of consolidating material dispersed throughout a suitable fluid carrier into an earthen formation for permeably consolidating such formation.
It can be appreciated that the present invention provides a new and improved method of consolidating incompetent sands in oil or fluid bearing formations.
The foregoing disclosure and description of the invention is illustrative and explanatory thereof and suitable variations may be made in the particular sequence of steps and the particular chemicals or compounds used within the scope of the appended claims without departing from the spirit of the invention.
What is claimed is:
1. A method of consolidating sand in a fluid producing earth formation, comprising the steps of: physically mixing an amount of consolidating solution with a nonmiscible oil having a viscosity at least as low as about that of diesel oil, whereby said consolidating solution is dispersed in said oil thereby forming a dispersion fluid; maintaining the dispersion fluid of the previous step; introducing said dispersion fluid into the sand formation desired to be consolidated; and, allowing the consolidating solution to set into a hard permeable mass.
2. The method of claim 1, wherein the formation to be treated is first cleaned with a mixture of diesel oil and a surfactant.
3. The method of claim 1, wherein the formation to be treated is first preflushed with a mud cleanout agent, and then secondly, cleaned with a mixture of diesel oil and a surfactant.
4. In a method of consolidating sand in a fluid producing earth formation, the sub-combination comprising the step of: introducing a dispersion fluid into the formation, said dispersion fluid being a physical mixture of a sodium silicate solution and a non-miscible oil having a viscosity at least as low as about that of diesel oil, wherein the sodium silicate solution is dispersed throughout the oil.
5. In a method of consolidating sand in a fluid producing earth format-ion, the sub-combination comprising the step of: introducing a dispersion fluid into the formation, said dispersion fluid being a physical mixture I of a liquid resin and a non-miscible oil having a viscosity at least as low as about that of diesel oil, wherein the liquid resin is dispersed throughout the oil. l
6. The method of claim 5, wherein the liquid resin is selected from the group consisting of phenolic resins and epoxy resins.
7. A method of consolidating sand in a fluid producing or hydrocarbon bearing earth formation, comprising the steps of: physically mixing a predetermined amount of sodium silicate solution with a non-miscible oil having .a viscosity at least as low as about that of diesel oil to which a dispersing agent has previously been added whereby the sodium silicate is dispersed throughout the oil to form a dispersion fluid; maintaining the sodium silicate solution dispersed in the oil; introducing the dispersion fluid into the formation to be treated; and, introducing a setting solution into the formation to set the sodium silicate While leaving some permeability in the formation so that fluid can be produced therefrom.
8. The method of claim 7, wherein the steps set forth therein are followed by the step of: introducing a setstabilizing material such as a calcium chloride solution into the formation for obtaining a strong set of the sodium silicate and stabilizing the same.
9. The method of claim 7, wherein said dispersing agent is selected from the group consisting of an oil soluble surfactant, and a mixture of an oil soluble surfactant and a substituted imidazolene.
10. A method of consolidating sand in a fluid producing earth formation, comprising the steps of: preparing a fluid dispersion of a liquid resin dispersed throughout a non-miscible oil having a viscosity at least as low as about that of diesel oil, a dispersing agent having been added to said non-miscible oil prior to said oil being mixed with said liquid resin; maintaining said liquid resin dispersed throughout said oil; introducing said dispersion fluid into the earth formation to be treated whereby a film of resin coating is deposited on the sand grains in the formation; and, allowing the resin to set into a hard permeable mass for permitting fluid flow therethrough.
11. The method of claim 10, wherein said dispersing agent is an oil soluble surfactant such as sorbitol sesqui tall oil.
12. The method of claim 10, wherein a suitable catalyst is added to said mixture of liquid resin and non-miscible oil for curing the resin after the resin has been introduced into the earthen formation.
13. The method of claim 10, wherein said dispersing agent is also a catalyst for curing the resin after the resin has been introduced into the earth formation.
14. The method of claim 13, wherein said catalyst and dispersing agent is a compound selected from the group consisting of diethylaminopropylamine and dimethylaminomethyl phenol.
15. The method of claim 10, wherein the formation to be treated is first cleaned with a mixture of diesel oil and a surfactant.
16. A method of consolidating sand in a fluid producing earth formation, comprising the steps of: physically mixing an amount of consolidating solution with a nonmiscible oil having a viscosity at least as low as about ten centipoise, at 77 F., whereby said consolidating solution is dispersed in said oil thereby forming a dispersion fluid; maintaining the dispersion fluid of the previous step; introducing said dispersion fluid into the sand formation desired to be consolidated; and, allowing the consolidating solution to set into a hard permeable mass.
17. In a method of consolidating sand in a fluid producing earth formation, the sub-combination comprising the step of: introducing a dispersion fluid into the formation, said dispersion fluid being a physical mixture of a sodium silicate solution and a non-miscible oil having a viscosity at least as low as about ten centipoise at 77 F., wherein the sodium silicate solution is dispersed throughout the oil.
18. In a method of consolidating sand in a fluid producing earth formation, the sub-combination comprising the step of: introducing a dispersion fluid into the formation, said dispersion fluid being a physical mixture of a liquid resin and a non-miscible oil having a viscosity at least as low as about ten centipoise at 77 F wherein the liquid resin is dispersed throughout the oil.
19. A method of consolidating sand in a fluid producing or hydrocarbon bearing earth formation, comprising the steps of: physically mixing a predetermined amount of sodium silicate solution with a non-miscible oil having a viscosity at least as low as about ten centipoise at 77 F. to which a dispersing agent has previously been added whereby the sodium silicate is dispersed throughout the oil to form a dispersion fluid; maintaining the sodium silicate solution dispensed in the oil; introducing the dispersion fluid into the formation to be treated; and,
9 introducing a setting solution into the formation to set the sodium silicate while leaving some permeability in the formation so that fluid can be produced therefrom.
20. A method of consolidating sand in a fluid .producing earth formation, comprising the steps of: preparing a fluid dispersion of a liquid resin dispersed throughout a non-miscible oil having a viscosity at least as low as about ten centipoise at 77 F.; a dispersing agent having been added to said non-miscible oil prior to said oil being mixed with said liquid resin, maintaining said liquid resin dispersed throughout said oil; and, introducing said dispersion fluid into the earth formation to be treated whereby a film of resin coating is deposited on the sand grains in the formation; and, allowing the resin to set into a hard permeable mass for permitting fluid flow therethrough.
References Cited by the Examiner UNITED STATES PATENTS 2,411,793 11/1946 Kennedy et a1. 166-33 2,770,306 11/1956 Clark 16633 2,946,747 7/1960 Kirkpatrick et al. 166-42 X 3,012,405 12/1961 Caron 16631 X 3,097,694 7/1963 Kerver 16629 X OTHER REFERENCES Marks Mechanical Engineers Handbook, sixth edition, McGraw-Hill Book Co., Inc., N.Y., 1958 (pp- 6-229 to 6-232).
Zaba and Doherty: Practical Petroleum Engineers Handbook, 3rd edition, Gulf Publishing Co., Houston, Texas, 1949 (page 599 relied on).
CHARLES E. OCONNELL Primary Examiner. S. I. NOVOSAD, Assistant Examiner.
UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No, 3, 291, 214 December 13, 1966 Wayne Fc Hower It is hereby certified that error appears in the above numbered patent requiring correction and that the said Letters Patent should read as corrected below.
Column 4, line 10, for "17/16 inches" read 1 7/16 inches column 5, line 19, for "H-p-cresol, 3%" read M-P Cresol 3 column 8 line 74, for "dispensed" read dispersed Signed and sealed this 19th day of September 1967 (SEAL) Attest:
EDWARD J. BRENNER Commissioner of Patents ERNEST W. SWIDER Attesting Officer
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|Citing Patent||Filing date||Publication date||Applicant||Title|
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|U.S. Classification||166/294, 166/295, 166/292|
|International Classification||C09K8/565, C09K8/56|