# Patent

## Title
Methods for producing a guar gum comprising undehusked guar and for using the guar gum in treating a subterranean formation

## Abstract

A method is provided for producing a guar gum powder, the method comprising the steps of: (a) flaking undehusked guar splits; and (b) grinding the flaked, undehusked guar splits to obtain guar gum powder. According to another aspect of the invention, a method is provided for treating a subterranean formation penetrated by a wellbore, the method comprises the steps of: (a) forming a treatment fluid, wherein the treatment fluid comprises: (i) an aqueous fluid; and (ii) a guar gum powder comprising at least 70% by weight gum material and at least 15% by weight husk material; and (b) introducing the treatment fluid into the subterranean formation through the wellbore, According to yet another aspect of the invention, the product of the method for producing a guar gum powder is used in the method for treating a subterranean formation.

## Background
CROSS-REFERENCE TO RELATED APPLICATIONS
Not applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable
REFERENCE TO MICROFICHE APPENDIX
Not applicable
FIELD OF THE INVENTION
The invention generally relates to methods for producing guar gum and to methods for using guar gum in treating a subterranean formation.
BACKGROUND OF THE INVENTION
Guar gum is widely used in the oil and gas industry in various well treatment procedures to increase production of oil and gas from a well. The general objective is, of course, to obtain oil and gas as a valuable commodity. Oil and gas is used in the production of products such as refined fuels and oils, and it is used also as the raw material for many types of plastics and chemicals.
Typically, oil and gas is found accumulated and trapped in various subterranean formations. The formations are considered to be subterranean regardless of whether they are under land or under water. For example, an oil and gas bearing subterranean formation may be offshore under a sea floor. To reach an oil and gas bearing subterranean formation, it is almost always necessary to drill a well many thousands of feet into the earth.
Drilling a well to reach one or more oil and gas bearing subterranean formations is merely one of the many challenges to bringing the oil and gas up to the surface. Another challenge is extracting the oil and gas from the subterranean formation. For example, the oil and gas may be trapped in the tiny pores in the rock of the subterranean formation, and the interconnections between the pores may be so few or poorly interconnected that it is difficult for the oil and gas to flow through the rock and into the well. Sometimes the formation is damaged by water being introduced into the formation by the mere drilling of the well into the formation, or by the water present in the drilling fluid used to drill the wellbore. Sometimes the formation is damaged by the migration of certain types of hydrocarbon, such as waxes. Sometimes the formation is damaged by the movement of tiny particles called “fines” that plug the interconnections between the pores in the rock. Thus, the permeability of the subterranean formation to the fluid flow of oil and gas is often very low. This presents another challenge to increase the flow of oil and gas through the rock of the subterranean formation and into the well. In the oil and gas industry, treatments performed to restore or enhance the productivity of a formation are referred to as “stimulation.”
Of the various stimulation techniques, one of the most common and widely accepted is hydraulic fracturing. In general, hydraulic fracturing involves injecting a fracturing fluid through the wellbore and into an oil and gas bearing subterranean formation at a sufficiently high rate of fluid flow and at a sufficiently high pressure to initiate and extend one or more fractures in the formation. To conduct hydraulic pressure through the wellbore, the fracturing fluid must be substantially incompressible. In addition, because of the large quantities of fracturing fluid required, the fracturing fluid is preferably based on readily-available and plentiful fluid. Thus, the typical fracturing fluid is based on water.
The fracturing fluid is injected through the wellbore at such a high flow rate and under such high pressure that the rock of the subterranean formation that is subjected to the hydraulic treatment cracks apart or fractures under the strain. When the formation fractures, the pressure is relieved as the fracturing fluid starts to move quickly through the fracture and out into the formation. The theoretical objective of forming such a fracture in the rock of the formation is to create a large surface area of the faces of the fracture. The large surface area allows oil and gas to flow from the rock of the subterranean formation into the facture, which provides an easy path for the oil and gas to easily flow into the well.
However, once the high pressure is relieved suddenly by the escape of the fracturing fluid through the created fracture and out further into the subterranean formation, the fracture has a tendency to be squeezed closed by the natural pressures on the rock within the deep subterranean formation. To keep the fracture open, some kind of material must be placed in the fracture to prop the faces of the fracture apart.
The desirable material for the purpose of propping the fracture apart must meet several criteria. For example, the material must have a sufficient strength not to be entirely crushed by the natural forces tending to push the fracture closed. The material must be capable of being fluidized so that it can flow with or immediately following the fracturing fluid. Additionally, the material also must itself not block or seal the fracture. Thus, a typical material used for the purpose of propping open a fracture is sand. Sand, in the aggregate, has a sufficiently high mechanical strength to prop open a fracture in a subterranean formation at typical depths and natural subterranean pressures; it can behave as a fluid in that it can be poured and flow; and the particles, even when tightly compacted, have a network of void spaces between them that can provide high porosity to fluid flow.
While sand is the most commonly used material for the purpose of propping the fracture open, many other materials of the appropriate size range and mechanical strength can be used. In the oil and gas industry, any suitable particulate material that is used for the purpose of propping open a fracture produced by hydraulic fracturing is called a “proppant.”
To be able to carry and place a proppant into a newly-created fracture, a fluid must have a sufficient viscosity to suspend and carry the proppant. In a low viscosity fluid, for example, the proppant would have a tendency to simply fall under gravity toward the bottom of the well instead of being carried with the fracturing fluid out into the newly-created fracture. For a fluid to be able to carry the proppant instead of having the proppant fall out of the fluid, the fracturing fluid needs to be made to have a much higher viscosity than that of water. Preferably, the fracturing fluid is a gel, which has a very high viscosity and great capacity for carrying a proppant suspended in the fluid.
Using a water-soluble gum is one of the ways to build viscosity in aqueous systems. Such a gum can be mixed with an aqueous fluid for use in a well to increase fluid viscosity. A sufficient concentration of the gum in an aqueous system can form a linear gel. Furthermore, the gum also can be crosslinked with other compounds, such as borates or various metals, to create a highly viscoelastic fluid, which is highly advantageous to transporting a proppant in a hydraulic fracturing procedure.
In the oil and gas industry, the gum conveniently is obtained in the form of a powder. The powder also can be suspended conveniently in a non-aqueous fluid, such as diesel, because the gum will not dissolve or swell with a non-aqueous fluid and being suspend in a non-aqueous fluid allows the gum powder to be handled as a liquid.
The oil and gas industry currently uses millions of pounds of gum per year to help build viscosity in aqueous systems, including for use in stimulation procedures such as hydraulic fracturing. The driving factor in selecting a source of gum for use in the oil and gas industry is cost.
Gum is found in certain seeds of Leguminosae, such as the seeds of the guar plant, the carob tree, the honey locust tree, and the flame tree. Among the available agricultural sources of gum, guar seed is one of the most economical.
The guar plant is drought resistant. The guar plant can be grown economically in semiarid regions of the world, such as India and Pakistan, where few other types of crops are viable. The guar plant grows about three to six feet in height and bears many beanlike pods, each which contains six to nine small, rounded guar seeds. In addition to being hardy, typical varieties of guar seed have a relatively high concentration of gum compared to gum-bearing seed from other Leguminosae.
The guar seed is composed of a germ (or embryo), a pair of endosperm sections, and a husk. The germ is brittle and relatively small compared to the endosperm sections. The germ is sandwiched between the pair of endosperm sections but easily separable from the endosperm sections. The endosperm sections contain mostly water-soluble gum (i.e., galactomannan polysaccharide) and minor amounts of proteinaceous material, inorganic salts, water insoluble gum, and cell membranes. The endosperm sections are tough and non-brittle. The endosperm sections are enclosed in the husk, which also is often referred to as the hull. The husk is very tough and very tightly associated with the endosperm sections. Typical varieties of guar seed have about 40%-46% by weight of the germ, about 38%-45% by weight of the endosperm sections (containing the gum), and about 14%-20% of the husk. Unless otherwise stated, all percentages are by weight, and, unless the context otherwise requires, on a dry basis.
However, processing guar seed into gum is mechanically challenging. In particular, it is difficult to separate the gum-containing endospern sections from the husk selectively.
The conventional process for extracting gum from guar seed includes splitting the seed, which splitting step is often termed “seed processing.” In splitting the seed, germ and undehusked guar splits are obtained. The undehusked guar splits are the endosperm sections with the husk still on them. The undehusked guar splits are extremely tough. As part of the splitting step, the brittle, relatively small germ is easily and substantially separated from the relatively large undehusked guar splits by particle size screening.
Next, the undehusked guar splits are processed conventionally in an attempt to separate the endosperm sections and the husk. This is done conventionally by passing the undehusked guar splits through an extruder having an elongated cylindrical barrel provided with an inlet opening, a die opening at the outlet end of the barrel, and a screw rotatable within the barrel to transport and work the undehusked guar splits. This step is sometimes referred to as “dehusking” or “dehulling” the undehusked guar splits. This step produces a product referred to as “dehusked guar splits” and “husk.” As part of the dehusking step, the dehusked guar splits and husk are separated by particle size screening.
The “dehusked guar splits” obtained from the conventional dehusking of undehusked guar splits are relatively large, mostly substantially in the form and shape of the endosperm sections, but still having bits of husk still attached to them. Thus, the “dehusked gaur splits” are actually not completely dehusked. Typically, dehusked guar splits comprise about 90% endosperm sections (w/w dry basis) wherein the husk has been substantially but not completely removed. Typically, the dehusked guar splits still contain about 10% husk material.
The “husk” obtained as a by-product from the conventional dehusking of undehusked guar splits is relatively small bits and pieces of husk material of various sizes and shapes. But, in the dehusking step, some of the endosperm material has also been removed with the husk and pieces of the endosperm material have been broken off from the endosperm sections. Thus, the “husk” is not only husk material, but includes bits and pieces of the endosperm sections. Typically, the “husk” comprises about 25-40% endosperm (containing the valuable gum), usually in the form of broken off pieces from the endosperm sections.
For example, after starting with a given amount of typical guar seed, in the splitting step, about 30% by weight is removed as germ. Then in the dehusking step, as much as an additional 37% by weight of the original amount of guar seed is removed as “husk.” The husk from the guar seed, however, includes substantial amounts of the endosperm. Typically, the husk comprises in the range of about 25% to about 40% by weight gum, and most typically about 30-35% by weight gum. Thus, the dehusking step removes about 10% to about 30% (typically 25%) by weight of the gum in the original amount of typical guar seed. Nevertheless, because of the difficulty in separation and the relatively low overall concentration of the endosperm material (i.e., gum) contained with the removed husk (i.e., less than about 30%), the husk obtained from conventional guar seed processing has low economic value and is usually considered to be a waste by-product, being typically sold for animal feed.
The dehusked guar splits are then flaked and ground into a powder. The dehusked splits are normally soaked in water from 30 minutes to several hours, at concentrations ranging from 80% to 120% by weight of splits relative to the amount of water, with 100% to 110% being preferred. Flaking is then accomplished by passing the wet dehusked guar splits between two counter rotating rollers, one roller moving substantially faster than the other, thus creating high levels of shear causing the wet splits to shred into moist fibers or flakes. Usually this process imparts such significant mechanical energy that part of the moisture is evaporated and the fiber/flakes heat up several degrees. The flakes are then passed through a hot air grinding or a hammer mill to reduce the flakes to a powder. Hot air is used to transport the flakes into the grinder, as well as to “flash dry cool” the particles during grinding. The temperature, humidity and mixture ratio of the air and flakes are such that the evaporative cooling during grinding offsets the heat generated from grinding so that it prevents the flakes and subsequently the ground powder from exceeding some designated maximum temperature. The powder typically ranges from about 10 microns to about 100 microns in average particle size. The powder is typically less than 10% water by weight and has a very stable and long shelf life. As previously mentioned, the guar gum powder is sometimes suspended in a non-aqueous fluid, such as diesel or environmentally friendly hydrocarbons, for storage and ease of handling.
When desired to be used, the powder is dispersed in water and allowed to hydrate. The viscosity of the solution depends in part on the concentration of the gum, usually in the range of about 0.05% to about 5% by weight of water, where 0.1% to 0.5% by weight of water, is the preferred range.
Despite the challenges in processing the gum from guar seed and the waste, guar gum is still one of the most common means with which to build viscosity in aqueous systems, especially for fracturing fluids (see, for example, U.S. Pat. Nos. 2,891,050 and 3,455,899). In general, it would be commercially valuable to be able to use more of the guar gum from guar seeds than conventional processing has allowed, including for applications outside the oil and gas industry.
SUMMARY OF THE INVENTION
According to one aspect of the invention, a method is provided for producing a guar gum powder, the method comprising the steps of: (a) flaking undehusked guar splits; and (b) grinding the flaked, undehusked guar splits to obtain guar gum powder.
According to another aspect of the invention, a method is provided for treating a subterranean formation penetrated by a wellbore, the method comprises the steps of: (a) forming a treatment fluid, wherein the treatment fluid comprising: (i) an aqueous fluid; and (ii) a guar gum powder comprising at least 70% by weight gum material and at least 15% by weight husk material; and (b) introducing the treatment fluid into the subterranean formation through the wellbore.
According to yet another aspect of the invention, the product of the method for producing a guar gum powder is used in the method for treating a subterranean formation.
These and other aspects of the invention will be apparent to one skilled in the art upon reading the following detailed description. While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof will be described in detail and shown by way of example. It should be understood, however, that it is not intended to limit the invention to the particular forms disclosed, but, on the contrary, the invention is to cover all modifications and alternatives falling within the spirit and scope of the invention as expressed in the appended claims.



BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying figures are incorporated into and form a part of the specification to illustrate examples of the prior art and the invention. These drawings together with the descriptions serve to explain the principles of the invention. The figures are only for illustrating the prior art and preferred and alternative examples of how the invention can be made and used and are not to be construed as limiting the invention to the illustrated and described examples. The various advantages and features of the invention will be apparent from a consideration of the drawing in which:
FIG. 1 outlines the prior art for conventionally processing guar seed;
FIG. 2 outlines a process according to one aspect of the invention for producing guar gum powder comprising the steps of flaking undehusked guar splits and grinding the flaked, undehusked guar splits;
FIG. 3 outlines a process according to a further embodiment of the invention that includes the step of hydrating the dehusked guar splits prior to flaking and drying the flaked, dehydrated guar splits prior to grinding;
FIG. 4 outlines a process according to a further embodiment of the invention that includes a step of particle size classification of the guar gum powder obtained from flaking and grinding undehusked guar splits;
FIG. 5 outlines a process according to a further embodiment of the invention that includes a step of separating at least some of the husk material from at least one of the classified guar gum powders obtained from flaking and grinding undehusked guar splits; and
FIG. 6 outlines a process according to another aspect of the invention for producing guar gum powder comprising the steps of flaking undehusked guar splits and separating at least some of the husk pieces or residue from the flaked, undehusked guar splits.



DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 outlines the conventional processing of guar seeds. The conventional processing includes splitting the guar seed, where the germ is separated from the guar seeds. The relatively small, brittle germ is easily separated from the relatively large undehusked guar splits by screening. Once the germ is removed, what is left is the undehusked guar splits.
Undehusked guar splits are attempted to be dehusked by a heating and abrasion process or via chemical treatments. The heating-abrasion process entails passing the de-germed splits through a heated rotating drum in which steam or direct flames are applied to the external surfaces of the drum. As the undehusked splits travel through the rotating drum, they are heated and become “plastic like”, while the thin layer of pericarp (husk skin) dries and shrinks, thus breaking (or partially breaking) its bond with the gum cotyledons. These hot “partially dehusked splits” are transferred to dehusking cylinders where fine toothed blades rotate with carefully controlled clearances from the cylinder walls. As the splits pass through these clearances, the husks are removed, along with fragments of the cotyledons, thus becoming the husk by-product that contains 25 to 40% gum.
A significant amount of the endosperm sections containing the desirable gum is lost in the dehusking step. When the undehusked guar splits are put through the dehusking step to remove the husk from the guar splits, pieces of the endosperm sections are also removed with the husk. These pieces of guar splits that are removed with the husk account for a significant loss of guar gum in guar seed processing, often 25 to 35% of total gum.
For example, starting with an original quantity of guar seed, typically about 30% by weight is removed as germ, and about 37% by weight is removed as husk, which includes a substantial amount of attached endosperm (the gum material), to produce only 29% by weight as dehusked guar splits for further processing into guar gum powder. Thus, in a conventional method for processing guar seed, about 37% by weight is wasted because the husk material was previously thought to be undesirable in a treatment fluid for use in well stimulation. Previous efforts have been to remove as much of the husk material as possible to produce relatively clean, dehusked guar splits for further processing into guar gum powder for use in viscosifying well treatment fluids.
According to one aspect of the invention, a method is provided for producing a guar gum powder, the method comprising the steps of: (a) flaking undehusked guar splits; and (b) hot air grinding the flaked, undehusked guar splits to obtain guar gum powder. FIG. 2 outlines a process according to this aspect of the invention for producing guar gum powder comprising the steps of flaking undehusked guar splits and grinding the flaked, undehusked guar splits. The undehusked guar splits are flaked and ground to form a guar gum powder that is approximately 50-65% gum. Preferably, the flaked, dehusked guar splits are ground into a fine powder having an average particle size normally ranging from 10 to 100 microns.
Thus, the method according to this aspect of the invention advantageously captures gum material that is normally lost during dehusking of the undehusked guar splits. For example, by omitting the dehusking step, typically an additional 25 to 30% of the gum from the guar seed can be used to produce guar gum powders according to the method of the invention. Thus, the invention can reduce procurement and raw material costs of gums by omitting the dehusking step, thereby recapturing the gum that would conventionally be discarded in the husk byproduct, thus providing a higher gum yield. If desired, the gum powder obtained using a method according to the present invention can be mixed with conventionally produced or “clean” guar gum powder without substantial amounts of husk residue material to obtain various intermediate grades of guar gum powders.
The methods according to the invention can further include the step of: splitting guar seed to obtain the undehusked guar splits and germ. The step of splitting the guar seed further comprises the step of separating the undehusked guar splits and the germ prior to the step of flaking.
The method of the invention also preferably comprises the step of washing the undehusked guar splits. The purpose of washing is to remove at least some of the fine particulate material from the undehusked guar splits. These small dust size particles prevent the flaking rollers from gripping the larger split pieces and imparting the high shear required to render functional viscosity when hydrated. The step of washing is with a washing solution, which can be any suitable washing fluid. Preferably, the washing fluid is an aqueous solution. As used herein, aqueous means water or a solution containing more than an unsubstantial amount of water.
The fine particles tend to float or be suspended in the aqueous solution and can be washed away from the undehusked guar splits by decanting the excess washing solution. The fine particles suspended in the washing solution also can be removed by screening the washing solution from the larger particles, for example, by using a screen mesh size that is smaller size than 25/+30. Also, agitating during the washing step can be helpful to remove at least some of the fine particulate from the undehusked guar splits.
It is believed that, by washing the fine particulate material from the undehusked guar splits, the undehusked guar splits are more effectively processed. Without being limited by theory, it is believed that, by removing the fine particulate from the undehusked guar splits, the undehusked guar splits have more frictional energy with the flaking rolls during the flaking step where frictional energy is used to rip the soaked and soft undehusked guar splits into shreds of stringy moist material, under very high shear rates. If the fine particulate is not removed from the undehusked guar splits, it is believed that the fine particulate lessen the frictional energy between the pieces and the flaking rolls, by serving as lubricants. By way of analogy, it is believed that the fine particulate act like tiny ball bearings between the surfaces of the flaking rolls and the undehusked guar splits.
The guar seed materials can be hydrated at any point in the process prior to flaking to provide a desired moisture content. For example, one such method involves pouring the water on the undehusked guar splits or adding the undehusked guar splits directly to the water and then agitating the guar splits continuously. Another method involves spraying and agitating the undehusked guar splits with a fine mist using an air pressure controlled atomizer.
According a presently most preferred embodiment of the invention, the method includes the step of: prior to flaking the undehusked guar splits, hydrating the undehusked guar splits. The step of hydrating the undehusked guar splits preferably further comprises: hydrating to a moisture content (wet basis) of about 35% to about 55% by weight. The step of hydrating the undehusked guar splits is preferably carried out at about 20° C. to about 80° C. over a period of time ranging from about 0.5 hour to about 2 hours. The step of hydrating the undehusked guar splits preferably further comprises: agitating the undehusked guar splits during the step of hydrating.
The step of hydrating comprises the step of soaking the undehusked guar splits. The soaking step is conducted in an aqueous soaking solution after the undehusked guar splits are washed. As used herein, aqueous means water or a solution containing more than an unsubstantial amount of water. It is believed that soaking in the presence of water hydrates or increases the moisture content in the undehusked guar splits, which is believed to make them easier to flake in the next step. Preferably, the step of soaking comprises soaking the undehusked guar splits under conditions sufficient to hydrate the guar pieces to a moisture content (wet basis) of about 35 to 55% by weight.
Preferably, the soaking solution is made up to be caustic. For example, in a most preferred embodiment, the soaking solution comprises sodium hydroxide, hydrogen chloride, and salts.
The step of soaking can be facilitated by mechanically agitating the undehusked guar splits in the soaking solution to promote mixing of the undehusked guar splits and the soaking solution. The mechanical agitation, for example, can be for periods of 30 minutes to several hours. Mechanical agitation can be accomplished through any means, such as with a ribbon blender.
If the undehusked guar splits are hydrated before flaking, the method preferably further comprising the step of: prior to the step of grinding, drying the flaked, undehusked guar splits. Preferably, the step of drying comprises drying the flaked, undehusked guar splits to a moisture content of less than 20% by weight. The drying step is preferably carried out in a dryer for about 10 to 15 minutes at about 80° C.-125° C. FIG. 3 outlines a process according to this further embodiment of the invention that includes the step of hydrating the dehusked guar splits prior to flaking and drying the flaked, dehydrated guar splits prior to grinding.
The undehusked guar splits can be transformed into a fine powder, generally with the steps outlined in FIGS. 3 and 6, including the steps of flaking and grinding, which are applied to produce a dry stable powder that can be useful in subterranean formations.
According to a presently most preferred embodiment of the invention, the step of flaking further comprises: high shear flaking. This type of flaking step generally entails passing the undehusked guar splits through high speed flattening rolls, where frictional energy is used to rip the undehusked guar splits into shreds or strings of moist material, a the volumetric average shear rate exceeding 5,000 l/sec.
According to the presently most preferred embodiment of the invention, the step of grinding comprises hot air grinding. This type of grinding step generally entails using a hot air hammer mill or pin mill. The grinding preferably grinds the flaked, undehusked guar splits into a fine powder, preferably having an average particle size ranging from about 10 to about 100 microns. The gum powder is relatively dry and stable for a long shelf life.
In the hot air grinding operation, it is preferable not to have completely dried the flaked, undehusked guar splits prior to grinding because it is believed that the operation of some moisture in the flaked, undehusked, guar splits helps keep the flaked material cool, as it is being ground so as to control the maximum temperature of the guar matter. In the hot air grinding operation, the moisture content from the previous soaking helps to control the maximum temperature of the guar gum, which reduces the risk to the guar gum from heat degradation. This is accomplished through evaporative cooling of the particles as the excess moisture “flashes” to vapor during the grinding. The grinding step transforms the flaked undehusked guar splits into a fine powder, normally ranging from 10 microns to 100 microns in average particle sizes. The undehusked guar splits are ground in hot air to form gum powder, which is dry and stable for a long shelf life. If desired, after grinding the gum powder can be dried further to help extend the shelf life of the product.
Additional steps can be used optionally to further process the powder of the guar gum, such as the particle size classification step, also known as the air classification or screening operation. Particle size classification can be accomplished by any particle sizing instrument. The particle size classification step is used to at least partially separate cellulose particles from gum particles, using specific gravity and/or size and/or shape, as the primary separation parameters. Alternatively, the cellulose particles are not separated from the gum particles.
The methods according to the invention preferably further comprise the step of: particle size classifying the guar gum powder to obtain classified guar gum powders. FIG. 4 outlines a process according to a further embodiment of the invention that includes a step of particle size classification of the guar gum powder obtained from flaking and grinding undehusked guar splits.
Further, when the step of particle size classification is included in a method according to the invention, the methods preferably further comprise the step of: separating at least some of the husk material from at least one of the classified guar gum powders. FIG. 5 outlines a process according to a further embodiment of the invention that includes a step of separating at least some of the husk material from at least one of the classified guar gum powders obtained from flaking and grinding undehusked guar splits.
If desired, the gum powder obtained in processes according to the present invention can be suspended in a non-aqueous solution, such as diesel or an “environmentally compatible hydrocarbon”, to carry the guar gum powder as a more-easily-handled liquid.
Additional steps can be used to further process the flaked, undehusked guar splits, such as “air classification” and/or the particle size classification step (also known as the screening operation step) to separate at least some of the cellulose (husk) pieces or particles from the gum particles. Alternatively, the cellulose particles are not separated from the gum particles prior to grinding.
Thus, according to a further aspect of the invention, after the step of flaking and before the step of hot air grinding, the methods can include the step of: separating at least some of the husk material from the flaked, undehusked guar splits. FIG. 6 outlines a process according to another aspect of the invention for producing guar gum powder comprising the steps of flaking undehusked guar splits and separating at least some of the husk pieces or residue from the flaked, undehusked guar splits.
It should also be understood, of course, that in this aspect of the invention as generally illustrated in FIG. 6, the method can further comprise the step of: particle size classifying the guar gum powder to obtain classified guar gum powders. Further according to this aspect of the invention, the method can further include the step of: separating at least some of the husk material from at least one of the classified guar gum powders.
The flaked, undehusked guar splits for use in the treatment methods according to the invention would typically and preferably comprise at least 30% by weight husk.
The methods of the invention optionally can comprise the step of agriculturally producing the guar seeds. In one preferred embodiment, the method comprises the step of producing guar seeds from Matador guar seeds. Matador is a specific plant variety protected in the United States by Plant Variety Protection Number: 200400235, issued Mar. 23, 2005 to Texas Tech University and Halliburton Energy Services, Inc. The Matador plant variety provides for a higher guar gum yield compared with guar seeds produced from typical varieties of guar plants.
The methods optionally can comprise splitting the guar seeds once the guar seeds are produced. Generally, the step of splitting is performed to substantially separate undehusked guar splits from the germ of the guar seeds, as previously explained.
According to yet another aspect of the invention, the invention includes the product of any of the methods according to the invention.
The method of the invention can comprise the further step of forming a well treatment fluid, wherein the well treatment fluid comprises an aqueous fluid and the powdered guar gum. The aqueous fluid, for example, can be fresh water, natural brines, and/or artificial brines. The artificial brines, for example, can be selected from the group consisting of potassium chloride solutions and sodium chloride solutions. Depending on the application, the well treatment fluid can include a variety of materials. For example, the well treatment fluid can include a proppant, a crosslinker, a breaker, etc. The well treatment fluid also can include a gel stabilizer, a delaying agent, etc.
The method can comprise the further step of introducing the well treatment fluid into the subterranean formation through the wellbore. In fracturing applications, the well treatment fluid can be introduced at a pressure sufficient to create at least one fracture in the formation. The method further can include the step of producing hydrocarbon from the wellbore.
According to the invention, a method for treating a subterranean formation penetrated by a wellbore is also provided. The method for treating a subterranean formation comprises the steps of: (a) forming a treatment fluid, wherein the treatment fluid comprises: (i) an aqueous fluid; and (ii) a guar gum powder comprising at least 70% by weight gum material and at least 15% by weight husk material; and (b) introducing the treatment fluid into the subterranean formation through the wellbore.
The water in the aqueous fluid serves to hydrate the guar gum powder. The aqueous fluid, for example, can be fresh water, natural brines, and/or artificial brines. The artificial brines, for example, can be selected from the group consisting of potassium chloride solutions and sodium chloride solutions.
In the treatment fluid, the guar gum powder preferably comprises in the range of about 0.05% to about 3% by weight of the treatment fluid.
Depending on the application, the treatment fluid can also include a variety of other materials. For example, the treatment fluid can include a proppant, a crosslinker, a breaker, etc. The treatment fluid can also include a gel stabilizer, a delayed release agent, etc.
According to the method of treating a subterranean formation, the step of introducing the treatment fluid further can comprise introducing the treatment fluid at a pressure sufficient to create at least one fracture in the formation.
Further according to the method of treating a subterranean formation, the method preferably further comprising the step of producing hydrocarbon from the wellbore.
Thus, the method provides synergy in using the both the gum and finely ground cellulose such that the material can be used in treating a subterranean formation in oil or gas wells. Without being limited by any theoretical explanation, it is believed that having finely ground husk particles in a guar gum powder, such as in a guar gum powder produced by a process according to the present invention, serves to help block fluid flow, and thus act to help control fluid loss. Therefore, the use of the guar husk material in a guar gum powder, which has in the past been thought of as being disadvantageous to treatment fluids, may actually advantageously effect the subterranean formation in certain applications by working to reduce fluid loss.
Possible applications that can benefit from the methods according to the invention for producing a guar gum powder having husk material therein include not only in applications of treatment of subterranean formations, but also a broad range of industrial applications. Such industries include, but are not limited to, foods, textiles, explosives, and stimulation procedures in the oil and gas industry, cosmetics, foods/pharmacy, paper, explosives, water treatment, mining petroleum, and paints.
Additional optional and desirable steps can be included in the method to obtain desirable guar gum products and the other by-products of processes according to the invention can have increased commercial value.
It can be appreciated in the art that a number of variations can be affected in washing, hydrating, flaking, drying, grinding, and classifying steps in accordance with the process described above without materially departing from the scope and spirit of the invention. Thus, the method of the invention can include additional steps that are not illustrated in FIGS. 2, 3, 4, 5, and 6. Such variations will be apparent to those skilled in the art and are to be included within the scope of this invention. For example, it should be understood by those skilled in the art that the method also can comprise the step of hydrating any whole seed or part thereof, including the guar splits, husk, or undehusked guar splits, at any point in the process to provide a desired moisture content.
After careful consideration of the specific and exemplary embodiments of the present invention described herein, a person of ordinary skill in the art will appreciate that certain modifications, substitutions, and other changes can be made without substantially deviating from the principles of the present invention. The detailed description is illustrative, the scope and spirit of the invention being limited only by the appended claims.

## Claims

1. A method for producing a guar gum powder, the method comprising the steps of:
a. flaking splits that consist essentially of undehusked guar splits; and
b. grinding the flaked, undehusked guar splits to obtain guar gum powder.

2. The method according to claim 1, further comprising the step of: splitting guar seed to obtain the undehusked guar splits and germ.

3. The method according to claim 2, where the step of splitting the guar seed further comprises the step of separating the undehusked guar splits and the germ prior to the step of flaking.

4. The method according to claim 2, further comprising the step of: agriculturally producing the guar seed.

5. The method according to claim 1, further comprising the step of: prior to flaking the undehusked guar splits, hydrating the undehusked guar splits.

6. The method according to claim 5, wherein the step of hydrating the undehusked guar splits further comprises: hydrating to a moisture content (wet basis) of about 35% to about 55% by weight.

7. The method according to claim 5, wherein the step of hydrating the undehusked guar splits is carried out at about 20° C. to about 80° C. over a period of time ranging from about 0.5 hour to about 2 hours.

8. The method according to claim 5, wherein the step of hydrating the undehusked guar splits further comprises: agitating the undehusked guar splits during the step of hydrating.

9. The method according to claim 5, further comprising the step of: prior to the step of grinding, drying the flaked, undehusked guar splits.

10. The method according to claim 9, wherein the step of drying comprises drying the flaked, undehusked guar splits to a moisture content of less than 20% by weight.

11. The method according to claim 9, wherein the drying step is carried out in a dryer for about 10 to 15 minutes at about 80° C.-125° C.

12. The method according to claim 1, wherein the step of flaking further comprises: high shear flaking.

13. The method according to claim 1, wherein the step of grinding comprises hot air grinding.

14. The method according to claim 1, further comprising the step of: particle size classifying the guar gum powder to obtain classified guar gum powders.

15. The method according to claim 14, further comprising the step of: separating at least some of the husk material from at least one of the classified guar gum powders.

16. The method according to claim 1, wherein the flaked, undehusked guar splits comprise at least 30% by weight husk.

17. The method according to claim 13, further comprising the step of: after the step of flaking and before the step of hot air grinding, separating at least some of the husk material from the flaked, undehusked guar splits.

18. The method according to claim 17, further comprising the step of: particle size classifying the guar gum powder to obtain classified guar gum powders.

19. The method according to claim 18, further comprising the step of: separating at least some of the husk material from at least one of the classified guar gum powders.

20. The product of the method according to claim 1.