Patent Application
20060180285
The present invention relates generally to natural cellulose fiber production, and particularly to fibrous products made from natural cellulose fibers obtained from rice straw.
With an availability of more than 580 million tons worldwide every year, rice straw is one of the most common sources of biomass available. Currently, there is very limited use of rice straw in construction, agriculture, paper, packing, fuel and energy industries. First, most of the rice straw available after harvest is either left on the ground or burnt. Tilling the straw left on the ground into the soil may be expensive. In addition, rice straw may have slow degradation rates, clogs field implements, is reported to harbor rice diseases and also inputs excess amounts of minerals into the soil. Although burning of rice straw is fast, economical and kills disease causing bacteria, the pollution generated by rice straw burning may pose a threat to the environment.
Although rice straw may be used for paper and fuel, such uses are associated with various limitations. For example, rice straw may include about 3 to 14% silica which has been reported to damage the pulping equipment when rice straw is used for paper. Further, with the existing technologies, using rice straw for ethanol or other fermentation products is not economical due to the possible low cellulose to glucose conversion rates. Thus, these limitations restrict the use of rice straw for industrial applications.
It is contemplated, however, that rice straw may have additional applications which remain to be fully explored. For example, rice straw may be used in fibrous applications such as composites and textiles. Industries using fibers are seeking a cheap and environmentally friendly alternative to the natural and synthetic fibers in current use due to several disadvantages associated with the production and use of these fibers. Natural fibers such as cotton need land, water and other natural resources to grow. Growing cotton may be environmentally unfriendly since such production often requires vast amounts of insecticide. Moreover, synthetic fibers are often from non-renewable petroleum resources. Further, synthetic fibers may consume more energy than that required to produce fibers from a renewable resource thereby making the process of synthetic fiber production environmentally unfriendly. Further, products made from synthetic fibers are difficult to be disposed after use. Thus, the need to find alternative sources for fibers, especially from the annually renewable resources, remains.
Agricultural byproducts such as cornhusks, corn stalks, pineapple and banana leaves, and coconut husks (coir fibers) have been used to extract natural cellulose fibers. However, not all of these byproducts may be used to produce fibers with properties required for high quality applications. The source, availability, composition and extraction conditions used to obtain the fibers influences the properties, processability and economics of fiber production. Coir fibers are coarse, have lower strength than most natural fibers but have high elongation. Coir is generally used for applications such as low value carpets, floor rugs and mats. Pineapple leaf and banana stems are available to a limited extent and require specific climate to grow. Producing fibers from these sources may not be economical. On the other hand, corn is the most widely grown crop in the world and the byproducts of corn production, cornhusks and corn stalks, are available in relatively large quantities and can be used to produce high quality fibers. Rice and wheat are also widely grown across the world and are second only to corn in terms of the worldwide production. Currently, no methods are known to be capable of producing high quality natural cellulose fibers from rice straw.
Rice straw generally contains about 35% cellulose, 30% hemicellulose, 15% lignin and about 20% ash. The cellulose fibers in rice straw are interconnected to each other to form large bundles with the widths of hundreds of micrometers to millimeters. They are then connected to each other by films. The ultimate fibers in rice straw are about 0.4 to 1.0 mm in length. These ultimate fibers are too short and/or too weak to be used for textile and other high value fibrous applications. To be classified as a textile fiber, the fiber should have a length at least 1000 times its' diameter with adequate tensile strength and elongation. For practical purposes, fiber length is required to be at least 1.0 cm and possess a strength greater than 1 gram per denier (denier is a common term used to describe the fineness or linear density of a textile material).
Although no methods are known to be capable of producing high quality natural cellulose fibers from rice straw, some methods used to obtain fibers from rice straw for paper and composite applications have been previously reported. For instance, a method of making boards from agricultural waste products including rice straw has been disclosed. In such instance, rice straw may be chopped into lengths of about ¼ to 1 inch in length and supplied to a steamer. The straw is steamed and refined in the steamer for approximately 5 to 30 seconds. A resin such as methyl diisocyanate is added into the steamed rice straw and the straw is then dried at about 350° F. The refined straw with a preferable moisture content of about 8 to 15% is fed into a mat forming press. The straw is pressed under a pressure of 400 to 800 psi with a temperature of about 400° F. The final boards made are about ½ inch in thickness. In addition to chopping the fibers into small lengths, the high temperature and pressure used in this process disintegrates the straw into small fibers that are unsuitable for textile and other high value fibrous applications.
An additional disclosure provides a method of producing pulp for paper from non-wood sources such as straw. In this method, the raw material is treated with about 10 to 30% of alkali solution based on the weight of the material with temperatures ranging from ambient to about 150° C. under pressures ranging from atmospheric to about 30 PSI for about 30 to 60 minutes. Fiber bundles are mechanically separated from the treated material and the dissolved substances called black liquor is removed. The alkali treated material is then treated with acids with or without chelating agents to remove metals. The pH of the solution is preferred to be in the range of 1.5 to 3 for this treatment. The acid treatment is carried out at ambient to 90° C. for 30 to 60 minutes. An ozone treatment may be given to the acid-treated material depending on the end use and brightness of the paper required. Typical ozone treatment is done using about 0.4 to 1.0% ozone on the weight of the fiber at temperatures of 25 to 30° C. for about 5 to 15 minutes. The pulp obtained after the ozone treatment may be bleached to obtain paper with the desired brightness. Again, however, the method described in this invention results in short and partially purified fibers that are unsuitable for textile and other high quality fibrous applications.
Therefore, it would be desirable to provide a method of production of high quality natural cellulose fibers from rice straw.
Accordingly, the present invention provides a process to produce high quality natural cellulose fibers from rice straw with properties similar to that of linen. Fibers here are defined as a bundle of single cells held together by lignin and other binding materials and hereafter referred to as “rice fibers”. Single cells are the smallest morphological units of cellulose in the straw and fibers. The rice fibers described here have the fineness, strength and elongation required for use in textiles, composites, and other high value applications. About 40 million tons of natural cellulose fibers world wide and more than a million ton of fibers in the United States of America may be produced every year by using 50% of the available rice straw. Producing fibers from rice straw may not only provide an environmentally friendly alternative to the natural and synthetic fibers currently in use, but may add value to the rice straw and benefit the farmers economically. In addition, this alternative use of rice straw may mitigate the problems associated with the burying or burning of rice straw.
In a first aspect of the present invention, a method of fiber extraction is provided. In the present aspect, the method may include treating rice straw with an alkali solution. For example, the alkali solution may be sodium hydroxide. Further, the method may include extracting coarse rice fibers from the rice straw and treating the extracted coarse rice fibers with an enzyme solution. For instance, the enzyme solution may include cellulase and a xylanase preparation.
In accordance with a further aspect of the present invention, extracted rice fibers that are at least 10 millimeters in length, no more than 0.5 millimeters in width and include a generally smooth surface are disclosed. In an aspect, a textile product including such extracted rice fibers is provided. For example, the textile product is at least one of yarn, woven material, non-woven material, apparel, carpet, automotive fabric, or a medical textile. In a further aspect, a composite including extracted rice fibers of at least 10 millimeters in length and no more than approximately 0.5 millimeters in width is provided.
In accordance with an additional aspect of the present invention, a fiber extraction kit is provided. In such aspect, the fiber extraction kit may include an alkali solution and an enzyme solution. In a preferred aspect, the alkali solution includes sodium hydroxide and the enzyme solution includes cellulase and a xylanase preparation. For instance, the alkali solution may include 1 N sodium hydroxide while the enzyme solution may include 1% cellulase and 1% xylanase (percentage being based upon the weight of the extracted rice fiber weight after alkaline treatment). Treatment of rice straw with the alkali solution followed by the enzyme solution allows rice fiber cells to be extracted from the rice straw. The kit may also include a washing solution for washing the rice straw following treatment with the alkali solution or the enzyme solution. Moreover, a neutralizing solution may also be included to neutralize any remaining alkali on the fibers following alkali treatment.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention as claimed. The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate an embodiment of the invention and together with the general description, serve to explain the principles of the invention.
The numerous advantages of the present invention may be better understood by those skilled in the art by reference to the accompanying figures in which:
Reference will now be made in detail to the presently preferred embodiments of the invention, examples of which are illustrated in the accompanying drawings.
Referring to
In an exemplary embodiment, the method 100 may include treating rice straw with an alkali solution 102. For example, the alkali solution includes sodium hydroxide (in anhydrous or liquid form). Alkali concentration used may depend on the quality of rice fiber required and also on the time and temperature of treatment. Preferable concentrations are between 0.1 to 5 N of sodium hydroxide or another alkali with the same alkalinity. The temperature of treatment varies with concentration and time of treatment. Preferable temperature is between 40° C. and 150° C. and most preferably below 100° C. to avoid degradation of the rice straw into singe cells or a bundle of single cells that are too small for high value applications. Duration of treatment is again dependent on the concentration of alkali and the temperature at which the treatment is carried out. Shorter treatment times at higher temperature and concentrations are preferred for practical reasons and for commercial application. Preferable duration is between 10 to 240 minutes with the most preferable duration between 20 and 60 minutes. The ratio of rice straw and alkali used for fiber extraction will also affect the quality and yield of the rice fibers produced. Alkali to material ratio of approximately 1:5 to 1:40 is suitable for rice fiber extraction, more preferably ratios are between approximately 1:5 and 1:25.
The process of alkaline extraction may be carried out in open baths, but preferably in a closed container and under atmospheric conditions to avoid oxidative degradation of rice straw fibers. The alkaline solution and the rice straws may be heated using any heating method. Preferably, the process is carried out in equipments having precise temperature control allowing more accurate temperature control. After the rice fiber extraction, the alkali may be purified and reused for further extraction, if desired. Such action may assist in minimizing the cost of extraction and disposal.
Following treatment with the alkali solution, the method 100 may include washing the treated fibers 104 with a wash solution (e.g., water) to remove the dissolved substances. In a preferred embodiment, the rice fibers are washed in cold water until the dissolved lignin and other materials are removed and clean rice fibers are obtained. Washing may be done in any suitable method as contemplated by one of ordinary skill in the art in order to remove impurities and dissolved substances, but not the desired rice fibers. Preferably, after washing, excess water is removed from the rice fibers by centrifugation or vacuum. Further, any remaining alkali in the rice fibers may be neutralized 106 by employing a dilute acid solution. Any acid including acetic acid may be used for neutralization. In an advantageous embodiment, 10% acetic acid is used with a liquid-to-fiber ratio of approximately at least 5:1 and preferably 10:1. The neutralized rice fibers may then be rinsed in water and dried 108. In an embodiment, the fibers are dried under ambient conditions (approximately 23° C.±2° C.) or at higher temperatures using hot air ovens, infrared driers or other drying methods. The drying time may vary depending upon the extent of moisture desired in the rice fibers. It is preferred that no liquid remain in order to prevent bacterial and fingal decomposition due to the presence of moisture.
Further, the method 100 may include extracting coarse rice fibers from the rice straw 110 and treating the extracted coarse rice fibers with an enzyme solution 112. For instance, the enzyme solution may include cellulase and a xylanase preparation. Enzymes in concentrations of approximately 0.1 to 10% on weight of the fiber may be employed for the treatments. The enzyme treatments may be carried out at ambient to approximately 60° C. for 20 to 1200 minutes with liquid to fiber ratio of 5:1 to 100:1. The pH of the solution may range from approximately 3.0 and 8.0. In an advantageous embodiment, the xylanase preparation is Pulpzyme® and the extracted coarse rice fibers are exposed to the enzyme solution for 40 minutes at 55° C. with a fiber to solution ratio of approximately 1:10 at a pH of approximately 6.0.
The method 100 provides a process of controlled delignification of the rice straw to remove the lignin and other interconnecting materials. The process also aids in partially removing the coloring matter in rice straw resulting in the formation of yellowish-white rice fibers. In such method, rice straws are treated with a preferred alkali concentration in the range of approximately 0.1 to 5 N at temperatures of approximately 40° C. to 150° C. The treatment times being between 10 to 240 minutes, preferably between 20 to 40 minutes for delignification to occur. Various chemicals that assist in delignification and rice fiber extraction such as sodium sulfite, sodium chlorites, chelating agents such as EDTA and some surfactants may also be used in the process. Rice fibers obtained after the alkali treatment are preferably subjected to an enzyme treatment to obtain finer and better quality fibers for the enzyme solution allows for further removal of lignin and other interconnecting materials.
In an embodiment, rice fibers obtained after the enzyme treatment may be washed in a wash solution (e.g., water) and dried 114 under ambient conditions (approximately 23° C.±2° C.). The resulting rice fibers are multicellular in which single cells are bonded together by lignin and other materials. In a further embodiment, the method 100 may include isolating single cells from the rice fibers 116 obtained after the alkaline and enzyme treatment. For example, single cells may be isolated by maceration. Such process may result in single cells with a length of approximately 0.6±0.15 millimeters and a width of 8.1±1.35 micrometers. The method 100 may also include analyzing the rice fibers 118 to determine fiber composition, morphology, and physical structure.
In accordance with an additional embodiment of the present invention, a fiber extraction kit is provided. In such embodiment, the fiber extraction kit may include an alkali solution and an enzyme solution. In a preferred embodiment, the alkali solution is a sodium hydroxide solution and the enzyme solution includes cellulase and a xylanase preparation. For instance, the alkali solution may include 1 N sodium hydroxide while the enzyme solution may include 1% cellulase and 1% xylanase such as Pulpzyme® (percentage being based upon the weight of the extracted rice fiber weight). Treatment of rice straw with the alkali solution followed by the enzyme solution allows rice fibers suitable for textile applications to be extracted from the rice straw. The kit may also include a washing solution (e.g., water) for washing the rice straw following treatment with the alkali solution or the enzyme solution and a neutralizing solution for neutralizing any remaining alkali on the rice fibers following alkali treatment.
Some of the specific examples in accordance with exemplary embodiments of the present invention are provided below.
Rice straw was treated with a sodium hydroxide at a concentration of 1N for 40 minutes at 100° C. with 5% of straw by weight in the alkali solution. The treated fibers were washed in water to remove the dissolved substances and the fibers formed were dried under ambient conditions. About 10% of the initial weight of rice straw used was obtained as high quality rice fibers after the alkali treatments.
Rice fibers obtained after the alkali treatments were treated with 1% (on weight of the fiber) each of Pulpzyme® and cellulase. The enzyme treatment was carried out at 55° C. for 40 minutes with 5% of the fibers in the enzyme solution at a pH of 6.0. Rice fibers obtained after the enzyme treatment were thoroughly washed in water and dried under ambient conditions. The properties of the high quality rice fibers obtained after the alkali and enzyme extraction are described in detail below.
Sodium carbonate of 2 N concentrations at boil for 90 minutes was used to extract rice fibers. The rice fibers obtained were washed in water, neutralized using 10% acetic acid. The rice fibers were rinsed in water and air-dried at ambient temperature. Rice fibers obtained were coarse and brownish yellow in color. Higher rice fiber yield of about 10 to 12% was obtained under these conditions. However, fiber quality measured by length, strength and other quality factors was reduced compared to fiber quality obtained after the sodium hydroxide and enzyme treatments.
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In addition to the quantitative determination of orientation of cellulose crystals in the fibers, the orientation of the crystals may be visually assessed from the patterns of the diffracting arcs in an X-ray diffraction picture. A long and diffuse diffracting arc may indicate a poorly oriented fiber whereas a sharp and bright diffraction arc means a fiber with oriented crystals.
Referring to
With continued reference to
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Rice straw is an economical, abundant and annually renewable source for natural cellulose fibers. For the first time, rice fibers with properties similar to that of linen have been produced using an economical and environmentally friendly process. Fibers obtained from rice straw have structure and properties similar to the common fibers in use for textiles. The composition, structure and properties of the rice fibers indicate that the fibers are suitable for most high quality fibrous applications. Rice fibers are probably suitable for blending with cotton, linen and other fibers to produce textiles and composites due to the similarities in structure and properties of rice fibers with the common cellulose fibers. Using rice straw for high quality fibrous applications may add value to the rice crops, mitigate concerns on the burning or disposing of rice straw and provide an environmentally friendly alternative to replace at least a part of the environmentally unfriendly natural and synthetic fibers currently in use.
It is contemplated that rice fibers may be used for apparels, home furnishings, automotive and medical textiles, carpets, and the like. Specific examples of products utilizing rice fiber obtained by the disclosed methods are provided.
Rice fibers obtained by the method 100 were processed on the conventional spinning machines. Rice fibers obtained from rice straw with an average of 20 denier were processed using a miniature spinning machinery. Rice fibers were hand blended with cotton in the weight ratio of 50/50. The rice fiber blends were processed through a modified card and drawframe to obtain the required grain sliver. All samples were carded twice for uniform mixing and parallelization of the rice fibers. Slivers from the drawframe were spun directly on a miniature sliver to yarn ring spinning machine. Parameters on the ring spinning machines were adjusted to obtain various counts of yarns. The finest yarns produced from 50/50 rice fiber/cotton blends were of 30 tex. The parameters used to process the rice fiber blends on the ring spinning machines are provided in
Various ratios of rice fibers were blended with cotton and processed on the open end spinning machines. The fibers were hand blended, processed on the card and drawframe to produce slivers. The silvers were spun into yarns on a Rieter open end spinning machine. The parameters that were used to produce various blends and counts of rice fiber/cotton yarns on the open end spinning machines are given in
Rice fibers with an average of 20 denier were hand blended with polyester in the weight ratio of 65% polyester to 35% rice fibers. The rice fiber blends were processed through a modified card and drawframe to obtain the required grain sliver. All samples were carded twice for uniform mixing and parallelization of the rice fibers. Slivers from the drawframe were spun directly on a miniature sliver to yarn ring spinning machine. Parameters on the ring spinning machines were adjusted to obtain various counts of yarns. The finest yarns produced from 65/35 polyester/rice fiber blends were of 27 tex. The properties of the polyester/rice fiber blended yarns were tested on standard yarn testing machines. Results show that the rice fiber blended yarns have similar strength and elongation compared to 65/35 polyester/cotton yarns produced using the conditions used to produce the rice fiber blended yarns.
Rice fibers with the structure and properties as described above were made into composites intended for use in the automotive headliner industry. Rice fibers in the ratio of 50 to 70% were blended with synthetic fibers such as polyester, polypropylene and polylactic acid. The fiber blend was carded to align the fibers. The carded web was then subject to a water lay process where the fibers become entangled to each other. The carded web is then dried and pressed at 200° C. for about 2 minutes. A composite with a thickness of about 3 to 4 mm was obtained by this process. In an advantageous embodiment, composites were produced from rice fibers blended with other synthetic fibers. Such embodiment was advantageous for it resulted in the production of composites with greater tensile strength and resiliency than composites produced from 100% synthetic fibers alone. It is contemplated that similar composites may be produced from 100% rice fibers and in other ratios of rice fibers with synthetic fibers or polymers.
In addition to the rice fibers and products from the high quality rice fibers, any product made using the short cellulose fibers and hemicellulose obtained as byproducts during rice fiber production are contemplated to be within the scope of the present invention.
It is believed that the present invention and many of its attendant advantages will be understood by the foregoing description. It is also believed that it will be apparent that various changes may be made in the form, construction and arrangement of the components thereof without departing from the scope and spirit of the invention or without sacrificing all of its material advantages. The form herein before described being merely an explanatory embodiment thereof. Further, it is to be understood that the claims included below are merely exemplary of the present invention and are not intended to limit the scope of coverage which has been enabled by the written description.
The present application claims the benefit under 35 U.S.C. §119(e) of U.S. Provisional Patent Application Ser. No. 60/648,335, entitled “High Quality and Long Natural Cellulose Fibers from Rice Straw and Method of Producing the Fibers,” filed Jan. 28, 2005 which is herein incorporated by reference in its entirety.
| Number | Date | Country | |
|---|---|---|---|
| 60648335 | Jan 2005 | US |
