CA2675940C - Basic sop process for recovery of oligosaccharides and polysaccharides from plants - Google Patents
Basic sop process for recovery of oligosaccharides and polysaccharides from plants Download PDFInfo
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- CA2675940C CA2675940C CA2675940A CA2675940A CA2675940C CA 2675940 C CA2675940 C CA 2675940C CA 2675940 A CA2675940 A CA 2675940A CA 2675940 A CA2675940 A CA 2675940A CA 2675940 C CA2675940 C CA 2675940C
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- sop
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/006—Pulping cellulose-containing materials with compounds not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Solid Oligosaccharides and Polysaccharides (SOP) are obtained from tissues of plants through the basic SOP process. A batch consisting of small pieces of plant tissue is soaked in alkaline solution at ambient temperature and pressure in a pulp-mill batch digester or similar extraction vessel. The alkaline extract is separated from the insoluble residue in the extraction vessel and transferred as clear solution to a SOP-forming tank, and the insoluble residue of plant tissue remaining in the extraction vessel is soaked in a second volume of alkaline solution. That second volume of alkaline extract is also transferred to a SOP-forming tank, whereupon the insoluble residue remaining in the extraction vessel is processed into pulp and paper or other products using established methods. SOP is produced in the SOP-forming tank as a coagulated suspension by adding to a volume of alkaline extract an equal volume of an aliphatic alcohol and mixing the two. SOP is concentrated, bleached and/or washed then dehydrated in a SOP separator. Alcohol used in the process is recovered by distillation, and the residual alkaline solution is adjusted to the desired concentration by addition of alkali then returned to the extraction vessel for treatment of another batch of plant tissue pieces. Potential uses of SOP are multi-faceted, e.g., as digestive fibre, foodstuff (e.g., syrup, sweetener), gum, paper additive, bulking agent in pharmacy or well-drilling, and as soluble carbohydrate for production of alcohol through fermentation or for other purposes including energy production.
Description
BASIC SOP PROCESS FOR RECOVERY OF OLIGOSACCHARIDES AND
POLYSACCHARIDES FROM PLANTS
Background of Invention The first man-made writing/drawing paper was produced by early Egyptians from the lowermost stem parts of papyrus, a sedge that grows up to 5 m in height, using a semi-pulping process involving stem slicing, pounding, cross-lapping and drying.
Thus, the word "paper" is derived from the Greek and Latin words papuros and papyrus, respectively.
The production of paper from papyrus was successful because of the natural ability of polysaccharides which are present in cell walls of all vascular plants to bond together upon drying, even when the plant tissue's adjoining fibres remained as discrete strips of tissue (i.e., not pulped). However, "true' paper is made from plant tissues that have been reduced to their individual fibres (i.e., fully pulped) and then re-constituted from a fibrous pulp suspension. (Hunter, D. 1947, Papermalcing, Dover Publications, New York).
True paper was being produced manually in China as early as the 2nd century BC, by manually pounding wetted cloth rags, bark of trees or shrubs, soft plant stems and leaves to a pulp, using a screen to lift the pulp out of the vat and produce a wet layer, followed by pressing moisture out of the wet layer and then hanging and drying that 'sheet' to produce paper. Papers of outstanding quality were produced from such plant tissues (Tsien, T.-H.
1973, Journal of the American Oriental Society 93:510). Centuries later, in 1800, the Great Seal Patent office, London, granted Matthias Koops a patent "...for a method of manufacturing paper from straw, hay, thistles, waste, and ruse of hemp and flax, and different kinds of wood and bark," again an indication that any tissue of any plant may serve for production of paper.
Wood as it occurs in trees and vascular plants in general is, in comparison to other plant tissues, a relatively hard bulky dark and inflexible material. Therefore, although wood is presently the dominant tissue of plants used in papermaking, woody stems were likely considered unsuitable as a material to be manually pounded into pulp at the outset of papermaking.
The first suggestion to utilize wood for paper-making may have been in 1719 by Rene Antoine Ferchault de Reaumur following his observations of the delicate papery nests created by American and Canadian wood wasps. Nevertheless, it was not until 1765 that Jacob Christian Schaffer made papers from pulp of beech, willow, aspen, mulberry, spruce and other woods, each paper being produced from wood pulp in admixture with rag fibres.
Schaffer also noted that wood treated with a lime paste required less time and energy to beat into pulp than untreated wood, and this evidently was the first step toward chemical pulping of wood.
The first paper made exclusively of wood pulp appears to have been a single page made of elm-wood fibres, produced in 1786 by Leorier Delisle and placed into a book authored by Charles Michel de Villette. In 1798 Nicolas-Louis Robert constructed a moving screen belt capable of receiving a continuous flow of suspended pulp and delivering an unbroken sheet of wet paper to a pair of squeeze rolls where most of the residual liquid was removed from the adjoining fibres. That innovation set the stage for mass production of paper hence the demand for larger quantities of pulp than could be produced manually. In 1840 Friedrich Keller secured a German patent for grinding logs against a millstone and, in 1867, ground-wood pulp was being produced in Massachusetts in order to make newsprint solely from wood fibres.
Newsprint as produced from chemically untreated ground wood was dull, darkened quickly and was not very strong, and the desire to produce stronger brighter paper from wood led to investigations into chemical pulping. The first chemical pulping of wood to operate on the industrial scale was the soda process, so-named because it used sodium hydroxide (NaOH) as the alkaline solution for cooking the wood pieces at elevated temperature and pressure. The soda process was developed in 1851 by Hugh Burgess and Charles Watt in England, and they secured a patent in the United States for the process in 1854. Alkaline sulfite pulping was patented in 1867 by Benjamin Tilghman in the United States, and Kraft pulping was patented in 1884 by Carl Dahl of Germany. Many variations on those chemical pulping processes have subsequently been described, and innumerable patents exist or existed in relation to their modifications. One variation presently invoking considerable interest is known as ASAM pulping (alkaline sulfite with anthraquinone and methanol as catalysts) as described by Patt and Kordsachia (1986, Das Papier 40 (10A):V1).
All chemical and related pulping processes are concerned with one or more direct or ancillary aspects involving treatment of wood particles with harsh chemicals at high temperature and pressure for many hours, the aim being to break the chemical bonds between cell-wall macromolecules such as lignin, hemicelluloses and cellulose in order that the individual plant cells, often referred to as 'fibers' in the pulping industry, can exist independently in suspension. The cell walls in non-woody plant tissues also contain hemicelluloses and cellulose but with little or no lignin present. Because chemical methods of wood pulping require the wood particles known as chips to be treated for several hours above atmospheric pressure at a temperature above the boiling point (approximately 100 C) of the cooking liquor, a generally massive pressure cooker known as a 'digester' is the starting point of industrial pulping. Under the conditions associated with cooking particles of plants with a high concentration of alkali at high temperature and a pressure above atmospheric within a digester, not only lignins but also hemicelluloses are hydrolyzed or otherwise chemically modified and released into the cooking liquor as smaller, soluble molecules.
The present invention embodies a practicable industrial process for obtaining a mixture of solid oligosaccharides and polysaccharides (SOP) in major quantity not only from raw wood but also from other plant tissues. The basic SOP process as specified and claimed herein may be implemented a s a pre-pulping sub-process carried out in a pulp-mill digester;
alternatively, it may operate independently of the pulping industry. The basic SOP process operates at atmospheric pressure, and the temperature of the alkaline solution soaking the plant tissue in the pulp-mill digester or other extraction vessel may be as low as 4 0C and in any case is kept below the boiling point in order to reduce hydrolytic breakdown of SOP
molecules.
POLYSACCHARIDES FROM PLANTS
Background of Invention The first man-made writing/drawing paper was produced by early Egyptians from the lowermost stem parts of papyrus, a sedge that grows up to 5 m in height, using a semi-pulping process involving stem slicing, pounding, cross-lapping and drying.
Thus, the word "paper" is derived from the Greek and Latin words papuros and papyrus, respectively.
The production of paper from papyrus was successful because of the natural ability of polysaccharides which are present in cell walls of all vascular plants to bond together upon drying, even when the plant tissue's adjoining fibres remained as discrete strips of tissue (i.e., not pulped). However, "true' paper is made from plant tissues that have been reduced to their individual fibres (i.e., fully pulped) and then re-constituted from a fibrous pulp suspension. (Hunter, D. 1947, Papermalcing, Dover Publications, New York).
True paper was being produced manually in China as early as the 2nd century BC, by manually pounding wetted cloth rags, bark of trees or shrubs, soft plant stems and leaves to a pulp, using a screen to lift the pulp out of the vat and produce a wet layer, followed by pressing moisture out of the wet layer and then hanging and drying that 'sheet' to produce paper. Papers of outstanding quality were produced from such plant tissues (Tsien, T.-H.
1973, Journal of the American Oriental Society 93:510). Centuries later, in 1800, the Great Seal Patent office, London, granted Matthias Koops a patent "...for a method of manufacturing paper from straw, hay, thistles, waste, and ruse of hemp and flax, and different kinds of wood and bark," again an indication that any tissue of any plant may serve for production of paper.
Wood as it occurs in trees and vascular plants in general is, in comparison to other plant tissues, a relatively hard bulky dark and inflexible material. Therefore, although wood is presently the dominant tissue of plants used in papermaking, woody stems were likely considered unsuitable as a material to be manually pounded into pulp at the outset of papermaking.
The first suggestion to utilize wood for paper-making may have been in 1719 by Rene Antoine Ferchault de Reaumur following his observations of the delicate papery nests created by American and Canadian wood wasps. Nevertheless, it was not until 1765 that Jacob Christian Schaffer made papers from pulp of beech, willow, aspen, mulberry, spruce and other woods, each paper being produced from wood pulp in admixture with rag fibres.
Schaffer also noted that wood treated with a lime paste required less time and energy to beat into pulp than untreated wood, and this evidently was the first step toward chemical pulping of wood.
The first paper made exclusively of wood pulp appears to have been a single page made of elm-wood fibres, produced in 1786 by Leorier Delisle and placed into a book authored by Charles Michel de Villette. In 1798 Nicolas-Louis Robert constructed a moving screen belt capable of receiving a continuous flow of suspended pulp and delivering an unbroken sheet of wet paper to a pair of squeeze rolls where most of the residual liquid was removed from the adjoining fibres. That innovation set the stage for mass production of paper hence the demand for larger quantities of pulp than could be produced manually. In 1840 Friedrich Keller secured a German patent for grinding logs against a millstone and, in 1867, ground-wood pulp was being produced in Massachusetts in order to make newsprint solely from wood fibres.
Newsprint as produced from chemically untreated ground wood was dull, darkened quickly and was not very strong, and the desire to produce stronger brighter paper from wood led to investigations into chemical pulping. The first chemical pulping of wood to operate on the industrial scale was the soda process, so-named because it used sodium hydroxide (NaOH) as the alkaline solution for cooking the wood pieces at elevated temperature and pressure. The soda process was developed in 1851 by Hugh Burgess and Charles Watt in England, and they secured a patent in the United States for the process in 1854. Alkaline sulfite pulping was patented in 1867 by Benjamin Tilghman in the United States, and Kraft pulping was patented in 1884 by Carl Dahl of Germany. Many variations on those chemical pulping processes have subsequently been described, and innumerable patents exist or existed in relation to their modifications. One variation presently invoking considerable interest is known as ASAM pulping (alkaline sulfite with anthraquinone and methanol as catalysts) as described by Patt and Kordsachia (1986, Das Papier 40 (10A):V1).
All chemical and related pulping processes are concerned with one or more direct or ancillary aspects involving treatment of wood particles with harsh chemicals at high temperature and pressure for many hours, the aim being to break the chemical bonds between cell-wall macromolecules such as lignin, hemicelluloses and cellulose in order that the individual plant cells, often referred to as 'fibers' in the pulping industry, can exist independently in suspension. The cell walls in non-woody plant tissues also contain hemicelluloses and cellulose but with little or no lignin present. Because chemical methods of wood pulping require the wood particles known as chips to be treated for several hours above atmospheric pressure at a temperature above the boiling point (approximately 100 C) of the cooking liquor, a generally massive pressure cooker known as a 'digester' is the starting point of industrial pulping. Under the conditions associated with cooking particles of plants with a high concentration of alkali at high temperature and a pressure above atmospheric within a digester, not only lignins but also hemicelluloses are hydrolyzed or otherwise chemically modified and released into the cooking liquor as smaller, soluble molecules.
The present invention embodies a practicable industrial process for obtaining a mixture of solid oligosaccharides and polysaccharides (SOP) in major quantity not only from raw wood but also from other plant tissues. The basic SOP process as specified and claimed herein may be implemented a s a pre-pulping sub-process carried out in a pulp-mill digester;
alternatively, it may operate independently of the pulping industry. The basic SOP process operates at atmospheric pressure, and the temperature of the alkaline solution soaking the plant tissue in the pulp-mill digester or other extraction vessel may be as low as 4 0C and in any case is kept below the boiling point in order to reduce hydrolytic breakdown of SOP
molecules.
The basic SOP process requires the availability of large volumes of an aliphatic alcohol such as methanol or ethanol in order to coagulate and further process the oligosaccharides and polysaccharides of SOP. Coincidentally, wood was used commercially as early as 1830 to produce methanol through the process of destructive distillation. In recent years, wood hemicelluloses have been identified as important substances for fermentative production of ethanol. Thus, there exists opportunity for the industry of the basic SOP
process to concomitantly operate a supporting process enabling it to be a producer rather than a consumer of the needed aliphatic alcohol(s).
Various patents related to ethanol production from sugars produced through hydrolysis of hemicelluloses have been filed in recent years. However, to the best of my knowledge none of those patents has addressed development of an industrial process such as described herein, for using aliphatic alcohol to obtain from alkaline extracts of woody or non-woody tissue of plants oligosaccharides and polysaccharides.
The use of an aliphatic alcohol to coagulate or "precipitate" polysaccharides in an alkaline solution gained acceptance as a routine scientific method, of common knowledge in the public domain, early in the 20th century (e.g., Norris, F.W. and Preece, I. A.
1930, Biochemistry Journal 24:59; Sands, L. and Gary, W. Y. 1933. Journal of Biological Chemistry 101:573; Adams, G.A. and Castagne, A.E. 1951, Canadian Journal of Chemistry 29:109).
Following upon that scientific advance, several patents were nevertheless awarded specifically in relation to use of an aliphatic alcohol, such as ethanol, to precipitate "hemicelluloses" from alkaline extracts of plant tissues. For example, U.S.
patent 3,935,022 for the manufacture of viscose products claimed "a process for removing hemicelluloses from hemicellulose-containing alkali solution consisting essentially of adding to said alkali solution a sufficient amount of a solvent consisting essentially of ethanol to precipitate hemicellulose from said alkali solution..." Similarly, U.S. patent 7,101,996 claimed "a process for the separation of purified hemicelluloses from insoluble cellulose and cellulose-hemicellulose complexes in caustic liquor from solubilizing fiber with alkali comprising the steps of adding alcohol to the caustic liquor to precipitate the hemicelluloses..." As noted, the supposed inventions underlying those claims were in the public domain well before the patent applications were filed, and more fundamentally the details of practicable industrial processes were not specified as such within those patents. In addition, there has been a tendency in the patent literature for the term 'hemicellulose' to be used without clear definition, although the meaning of the term can be more rigorously interpreted. (Aspinall, G. 0. 1970, Polysaccharides. Pergamon Press, Oxford; Wilkie, K.C.B. 1985, pp 1-37, in Biochemistry of Plant Cell Walls, edited by C.T. Brett and J. R. Hillman, Cambridge U. Press).
As noted by Wilkie (1985, p 3 in Biochemistry of Plant Cell Walls, edited by C.T. Brett and J. R.
Hillman, Cambridge U. Press), "Confusion and uncertainty is caused when terms are used that are ill-defined or, as in the case of hemicelluloses, when terms have considerable, and unrecognized, variability in their definition." Recognizing that the oligosaccharides and polysaccharides of the SOP process have their origin in native hemicelluloses (in agreement with the fact that cotton fibres, known to contain almost pure cellulose, yield almost no SOP
within the basic SOP process) which are well established to comprise a variable, large and incompletely known number of oligosaccharides, oligosaccharide derivatives, polysaccharides and polysaccharide derivatives, the process taught here deliberately avoids referring to them as hemicelluloses.
The embodiments of the basic SOP process require that a distinction be made between the natural hemicelluloses and the oligosaccharides and polysaccharides obtained by the SOP
process. Aqueous alkaline treatment of plant tissues not only hydrolyzes into smaller molecules those polysaccharides referred to as hemicelluloses but also saponifies the natural esters (e.g., acetyl or diferulyl groups) natural to those polysaccharides. In other words, alkali extraction changes the true or 'native' polysacchardies of plants into de-esterified polysaccharides and shorter oligosaccharides differing in both chemical properties and chain length from those occurring naturally. (Neilson, M.J. and Richards, G.
N. 1978, Journal of the Science of Food and Agriculture 29:513). One way to understand the distinction is to consider the solubility of native hemicelluloses vis-d-vis solid oligosaccharides and polysaccharides obtained by the basic SOP process. In general native hemicelluloses are not misicible in water and will produce a cloudy suspension rather than a clear solution when mixed with cool or lukewarm water. SOP, on the other hand, upon mixing with water at sub-ambient or higher temperature, readily provides a clear solution of oligosaccharides and polysaccharides. Dialysis using M.W. 10,000 cut-off has nevertheless revealed that the molecules in the clear solution are miscible in water. In other words, the colligative properties of SOP are different from those of native hemicelluloses.
In developing this invention referred to as the basic SOP process, a variety of woody and non-woody plant species was investigated. Based on the findings, it is suggested that all plants will yield some amount of SOP when subjected to the basic SOP process.
However, the yield clearly varies among species, with Magnoliophyta in general providing more SOP
than Coniferophyta. Of the species investigated, bamboo stems yielded the most SOP, raw fibres from cotton bolls the least. It is apparent from Table 12 in the example given that common roadside weeds may be excellent sources of SOP.
Potential end uses of SOP are not the subject of this Specification because those end uses remain to be determined and are expected to vary depending on the plant species and tissue used to produce the SOP. In general, SOP is expected to be useful in a variety of applications including production of novel kinds of paper, as sizing or other paper additive, as digestive fiber, as chewing and other gums, as foodstuffs (e.g., syrup, sweetener) for both animals and humanity, as a bulking agent in pharmacy, as carbohydrate in support of fermentation, and for energy production.
The novelty of the SOP process goes beyond linking together a series of existing technologies in the correct sequence needed to provide large quantities of SOP
for use in various commercial production streams. In relation to wood pulping, the black liquor issuing from the digester after processing wood chips contains not only sulfonated lignin derivatives but also sulfonated and otherwise chemically modified compounds derived from the hemicellulose fraction (Niemela, K. 1990. Annales Academiae Scientiarum Fennicae, Series A, II. Chemica 229). By removing soluble and/or miscible oligosaccharides and polysaccharides from wood chips at the beginning of the pulping process, a significant fraction of the biomass is prevented from contributing to the black liquor stream and, additionally, the remaining wood chips are effectively primed with alkali from the SOP
soak(s) enabling subsequent pulping to proceed more efficiently. In relation to tissues from plants not classified as trees, such as agricultural plants, weeds, bamboos, and also bark and other tissues of trees, although all were established ages ago to be useful sources of pulp particularly for production of high quality grades of paper in industrial pulping those species have been supplanted by trees primarily because of the ready availability of massive quantities of more or less uniform wood tissue within tree stems. However, the SOP process adds a new dimension to the utilization of non-wood plant tissues, as it enables production of both SOP and useful pulp-and-paper fibres in a sequential process regardless of the plant species.
DETAILED DESCRIPTION
The basic SOP process claimed herein produces solid oligosaccharides and polysaccharides from natural chemical substances resident within tissues of plants. The process begins in any extraction vessel capable of being loaded with and containing pieces of raw plant tissue and primary soaking solution. These pieces of raw plant tissue may be of dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length. Within those dimensional constraints, the precise thickness, width and length of said pieces of raw plant tissue loaded into said extraction vessel are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Although said basic SOP process does not require a pulp-mill digester to serve as said extraction vessel, said basic SOP process can readily be accomplished as the first phase of the overall pulping process as carried out within a pulp-mill digester, particularly if said digester is used for soda, alkaline sulfite, Kraft or ASAM chemical, semi-chemical or chemi-mechanical pulping. Performing said basic SOP process in association with pulping enables more complete utilization of said pieces of raw plant tissue, increase in overall yield of economically useful products, and reduction in the amount of substances contributing to the so-called "black liquor" resulting from the so-called "cook" done in the pulp-mill digester at above ambient pressure and elevated temperature in order to convert the raw plant tissue into its individual fibres.
process to concomitantly operate a supporting process enabling it to be a producer rather than a consumer of the needed aliphatic alcohol(s).
Various patents related to ethanol production from sugars produced through hydrolysis of hemicelluloses have been filed in recent years. However, to the best of my knowledge none of those patents has addressed development of an industrial process such as described herein, for using aliphatic alcohol to obtain from alkaline extracts of woody or non-woody tissue of plants oligosaccharides and polysaccharides.
The use of an aliphatic alcohol to coagulate or "precipitate" polysaccharides in an alkaline solution gained acceptance as a routine scientific method, of common knowledge in the public domain, early in the 20th century (e.g., Norris, F.W. and Preece, I. A.
1930, Biochemistry Journal 24:59; Sands, L. and Gary, W. Y. 1933. Journal of Biological Chemistry 101:573; Adams, G.A. and Castagne, A.E. 1951, Canadian Journal of Chemistry 29:109).
Following upon that scientific advance, several patents were nevertheless awarded specifically in relation to use of an aliphatic alcohol, such as ethanol, to precipitate "hemicelluloses" from alkaline extracts of plant tissues. For example, U.S.
patent 3,935,022 for the manufacture of viscose products claimed "a process for removing hemicelluloses from hemicellulose-containing alkali solution consisting essentially of adding to said alkali solution a sufficient amount of a solvent consisting essentially of ethanol to precipitate hemicellulose from said alkali solution..." Similarly, U.S. patent 7,101,996 claimed "a process for the separation of purified hemicelluloses from insoluble cellulose and cellulose-hemicellulose complexes in caustic liquor from solubilizing fiber with alkali comprising the steps of adding alcohol to the caustic liquor to precipitate the hemicelluloses..." As noted, the supposed inventions underlying those claims were in the public domain well before the patent applications were filed, and more fundamentally the details of practicable industrial processes were not specified as such within those patents. In addition, there has been a tendency in the patent literature for the term 'hemicellulose' to be used without clear definition, although the meaning of the term can be more rigorously interpreted. (Aspinall, G. 0. 1970, Polysaccharides. Pergamon Press, Oxford; Wilkie, K.C.B. 1985, pp 1-37, in Biochemistry of Plant Cell Walls, edited by C.T. Brett and J. R. Hillman, Cambridge U. Press).
As noted by Wilkie (1985, p 3 in Biochemistry of Plant Cell Walls, edited by C.T. Brett and J. R.
Hillman, Cambridge U. Press), "Confusion and uncertainty is caused when terms are used that are ill-defined or, as in the case of hemicelluloses, when terms have considerable, and unrecognized, variability in their definition." Recognizing that the oligosaccharides and polysaccharides of the SOP process have their origin in native hemicelluloses (in agreement with the fact that cotton fibres, known to contain almost pure cellulose, yield almost no SOP
within the basic SOP process) which are well established to comprise a variable, large and incompletely known number of oligosaccharides, oligosaccharide derivatives, polysaccharides and polysaccharide derivatives, the process taught here deliberately avoids referring to them as hemicelluloses.
The embodiments of the basic SOP process require that a distinction be made between the natural hemicelluloses and the oligosaccharides and polysaccharides obtained by the SOP
process. Aqueous alkaline treatment of plant tissues not only hydrolyzes into smaller molecules those polysaccharides referred to as hemicelluloses but also saponifies the natural esters (e.g., acetyl or diferulyl groups) natural to those polysaccharides. In other words, alkali extraction changes the true or 'native' polysacchardies of plants into de-esterified polysaccharides and shorter oligosaccharides differing in both chemical properties and chain length from those occurring naturally. (Neilson, M.J. and Richards, G.
N. 1978, Journal of the Science of Food and Agriculture 29:513). One way to understand the distinction is to consider the solubility of native hemicelluloses vis-d-vis solid oligosaccharides and polysaccharides obtained by the basic SOP process. In general native hemicelluloses are not misicible in water and will produce a cloudy suspension rather than a clear solution when mixed with cool or lukewarm water. SOP, on the other hand, upon mixing with water at sub-ambient or higher temperature, readily provides a clear solution of oligosaccharides and polysaccharides. Dialysis using M.W. 10,000 cut-off has nevertheless revealed that the molecules in the clear solution are miscible in water. In other words, the colligative properties of SOP are different from those of native hemicelluloses.
In developing this invention referred to as the basic SOP process, a variety of woody and non-woody plant species was investigated. Based on the findings, it is suggested that all plants will yield some amount of SOP when subjected to the basic SOP process.
However, the yield clearly varies among species, with Magnoliophyta in general providing more SOP
than Coniferophyta. Of the species investigated, bamboo stems yielded the most SOP, raw fibres from cotton bolls the least. It is apparent from Table 12 in the example given that common roadside weeds may be excellent sources of SOP.
Potential end uses of SOP are not the subject of this Specification because those end uses remain to be determined and are expected to vary depending on the plant species and tissue used to produce the SOP. In general, SOP is expected to be useful in a variety of applications including production of novel kinds of paper, as sizing or other paper additive, as digestive fiber, as chewing and other gums, as foodstuffs (e.g., syrup, sweetener) for both animals and humanity, as a bulking agent in pharmacy, as carbohydrate in support of fermentation, and for energy production.
The novelty of the SOP process goes beyond linking together a series of existing technologies in the correct sequence needed to provide large quantities of SOP
for use in various commercial production streams. In relation to wood pulping, the black liquor issuing from the digester after processing wood chips contains not only sulfonated lignin derivatives but also sulfonated and otherwise chemically modified compounds derived from the hemicellulose fraction (Niemela, K. 1990. Annales Academiae Scientiarum Fennicae, Series A, II. Chemica 229). By removing soluble and/or miscible oligosaccharides and polysaccharides from wood chips at the beginning of the pulping process, a significant fraction of the biomass is prevented from contributing to the black liquor stream and, additionally, the remaining wood chips are effectively primed with alkali from the SOP
soak(s) enabling subsequent pulping to proceed more efficiently. In relation to tissues from plants not classified as trees, such as agricultural plants, weeds, bamboos, and also bark and other tissues of trees, although all were established ages ago to be useful sources of pulp particularly for production of high quality grades of paper in industrial pulping those species have been supplanted by trees primarily because of the ready availability of massive quantities of more or less uniform wood tissue within tree stems. However, the SOP process adds a new dimension to the utilization of non-wood plant tissues, as it enables production of both SOP and useful pulp-and-paper fibres in a sequential process regardless of the plant species.
DETAILED DESCRIPTION
The basic SOP process claimed herein produces solid oligosaccharides and polysaccharides from natural chemical substances resident within tissues of plants. The process begins in any extraction vessel capable of being loaded with and containing pieces of raw plant tissue and primary soaking solution. These pieces of raw plant tissue may be of dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length. Within those dimensional constraints, the precise thickness, width and length of said pieces of raw plant tissue loaded into said extraction vessel are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Although said basic SOP process does not require a pulp-mill digester to serve as said extraction vessel, said basic SOP process can readily be accomplished as the first phase of the overall pulping process as carried out within a pulp-mill digester, particularly if said digester is used for soda, alkaline sulfite, Kraft or ASAM chemical, semi-chemical or chemi-mechanical pulping. Performing said basic SOP process in association with pulping enables more complete utilization of said pieces of raw plant tissue, increase in overall yield of economically useful products, and reduction in the amount of substances contributing to the so-called "black liquor" resulting from the so-called "cook" done in the pulp-mill digester at above ambient pressure and elevated temperature in order to convert the raw plant tissue into its individual fibres.
Said primary soaking solution consists of a known concentration, ranging from 0.5 - 10 M, of an alkaline hydroxide in aqueous solution, and said primary soaking solution is provided to said extraction vessel in sufficient or greater volume needed to achieve a soak, here designated as primary soak, of all said pieces of raw plant tissue in said extraction vessel for the full duration of primary soaking time selected from within the range 0.1 -4.0 hours at a temperature selected from within the range 4 - 100 C. The species of said alkaline hydroxide may be lithium hydroxide, potassium hydroxide or sodium hydroxide.
The species and concentration of said alkaline hydroxide, the precise duration of said primary soaking time, and the precise temperature(s) of said primary soaking solution used during said primary soaking time are, within the stated bounds, variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said primary soaking time, said primary soaking solution is displaced from the insoluble residue of said pieces of raw plant tissue remaining in said extraction vessel using gravity flow, positive pressure or vacuum expulsion to expel the recoverable volume of said primary soaking solution, here designated as primary recoverable volume, into conduit(s) running from said extraction vessel to SOP-forming tank. Said primary recoverable volume is transferred within said conduit(s) from said extraction vessel into said SOP-forming tank using valves and pumps as necessary. Said primary recoverable volume is retained in said SOP-forming tank until the temperature of the liquid of said primary recoverable volume is measured to be at or below 40 oC, hereafter designated as ambient temperature.
Said SOP-forming tank operates at ambient pressure (i.e., the pressure of the surrounding air) and said ambient or lower temperature and is equipped with several devices, viz., a device for accurately measuring and indicating the volume of contained liquid within said SOP-forming tank, a refrigeration unit for cooling the internal environment, with thermometers for accurately measuring the temperature of said contained liquid and air above said contained liquid, with mechanism(s) to stir and/or mix said contained liquid, with intake and outlet ports and pumps for receiving and discharging liquids and fluid suspensions, respectively, and with devices needed to regulate rates of stirring and/or mixing, receiving and discharging of both incoming liquids and outward flowing suspensions. The precise operating temperature of said SOP-forming tank is a variable which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
An aliphatic alcohol in liquid state of at least 95% purity and containing by volume 5% or less water, and pre-chilled to a temperature at least 10 0C below its flash point is transferred within conduit(s), using valves and pumps as necessary, from an alcohol storage tank into said SOP-forming tank containing said primary recoverable volume. Suitable species of said aliphatic alcohol include ethanol, methanol, 2-propanol or n-butanol. Said aliphatic alcohol is added to said primary recoverable volume until the total volume of liquid contained in said SOP-forming tank is twice, within volumetric precision of 2%, that of said primary recoverable volume. Said total volume of liquid contained in said SOP-forming tank is mixed for a time, here designated as primary mixing time, selected from the range 1 - 30 minutes, the duration of said primary mixing time being sufficient to achieve uniform mixing thus producing a 1:1 (v/v) homogeneous mixture, here designated as primary mixture, of said primary recoverable volume and the equivalent volume of said aliphatic alcohol. After elapse of said primary mixing time, said primary mixture is held static at said ambient temperature and said ambient pressure in said SOP-forming tank for a setting time, here designated as primary setting time, selected from the range 0.1 - 24 hours. During the course of said primary setting time, a fluid suspension of coagulated substances containing oligosaccharides and polysaccharides, and here designated as primary suspension, forms.
The species of said aliphatic alcohol, the precise duration of said primary mixing time and the precise duration of said primary setting time are, within the stated bounds, variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
After elapse of said primary setting time, said primary suspension in said SOP-forming tank is stirred or mixed continuously for a time, here designated as primary stirring time, at said ambient temperature and said ambient pressure to produce a dispersed primary suspension.
The species and concentration of said alkaline hydroxide, the precise duration of said primary soaking time, and the precise temperature(s) of said primary soaking solution used during said primary soaking time are, within the stated bounds, variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said primary soaking time, said primary soaking solution is displaced from the insoluble residue of said pieces of raw plant tissue remaining in said extraction vessel using gravity flow, positive pressure or vacuum expulsion to expel the recoverable volume of said primary soaking solution, here designated as primary recoverable volume, into conduit(s) running from said extraction vessel to SOP-forming tank. Said primary recoverable volume is transferred within said conduit(s) from said extraction vessel into said SOP-forming tank using valves and pumps as necessary. Said primary recoverable volume is retained in said SOP-forming tank until the temperature of the liquid of said primary recoverable volume is measured to be at or below 40 oC, hereafter designated as ambient temperature.
Said SOP-forming tank operates at ambient pressure (i.e., the pressure of the surrounding air) and said ambient or lower temperature and is equipped with several devices, viz., a device for accurately measuring and indicating the volume of contained liquid within said SOP-forming tank, a refrigeration unit for cooling the internal environment, with thermometers for accurately measuring the temperature of said contained liquid and air above said contained liquid, with mechanism(s) to stir and/or mix said contained liquid, with intake and outlet ports and pumps for receiving and discharging liquids and fluid suspensions, respectively, and with devices needed to regulate rates of stirring and/or mixing, receiving and discharging of both incoming liquids and outward flowing suspensions. The precise operating temperature of said SOP-forming tank is a variable which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
An aliphatic alcohol in liquid state of at least 95% purity and containing by volume 5% or less water, and pre-chilled to a temperature at least 10 0C below its flash point is transferred within conduit(s), using valves and pumps as necessary, from an alcohol storage tank into said SOP-forming tank containing said primary recoverable volume. Suitable species of said aliphatic alcohol include ethanol, methanol, 2-propanol or n-butanol. Said aliphatic alcohol is added to said primary recoverable volume until the total volume of liquid contained in said SOP-forming tank is twice, within volumetric precision of 2%, that of said primary recoverable volume. Said total volume of liquid contained in said SOP-forming tank is mixed for a time, here designated as primary mixing time, selected from the range 1 - 30 minutes, the duration of said primary mixing time being sufficient to achieve uniform mixing thus producing a 1:1 (v/v) homogeneous mixture, here designated as primary mixture, of said primary recoverable volume and the equivalent volume of said aliphatic alcohol. After elapse of said primary mixing time, said primary mixture is held static at said ambient temperature and said ambient pressure in said SOP-forming tank for a setting time, here designated as primary setting time, selected from the range 0.1 - 24 hours. During the course of said primary setting time, a fluid suspension of coagulated substances containing oligosaccharides and polysaccharides, and here designated as primary suspension, forms.
The species of said aliphatic alcohol, the precise duration of said primary mixing time and the precise duration of said primary setting time are, within the stated bounds, variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
After elapse of said primary setting time, said primary suspension in said SOP-forming tank is stirred or mixed continuously for a time, here designated as primary stirring time, at said ambient temperature and said ambient pressure to produce a dispersed primary suspension.
, Said primary stirring time is whatever length of time is required to transfer the entire volume of said dispersed primary suspension generated from said primary recoverable volume and the equivalent volume of added said aliphatic alcohol out of said SOP-forming tank, conveying it using pumps as necessary from said SOP-forming tank at a controlled flow rate within non-valved conduit(s) to the inlet of a device, here designated as SOP
separator, operating at said ambient or lower temperature and said ambient or lower pressure and capable of performing the processes of separating SOP from liquid, retaining and accumulating cakes of primary SOP, and concomitantly expelling liquid here designated as primary waste solution from said SOP separator. Said process of separating SOP from liquid, retaining and accumulating said cakes of primary SOP, and concomitantly expelling said primary waste solution requires use in said SOP separator of a filter and backing support, this filter and backing support here designated as SOP
filter. Said SOP
filter must be cellulose based and must not retain particles smaller than 1.0 um.
Said controlled flow rate of said dispersed primary suspension from said SOP-forming tank into said SOP separator is adjusted to be equal to or less than that of the outflow rate from said SOP separator of said primary waste solution. Said controlled flow rate is to ensure that said dispersed primary suspension within said conduit(s) between said SOP-forming tank and said SOP separator is maintained as nearly as possible as a uniformly dispersed suspension during its inflow into said SOP separator. Said primary waste solution upon exiting said SOP separator is transferred within conduit(s), using pumps and valves as necessary, to a storage tank in support of its subsequent distillation, said distillation being to recover said aliphatic alcohol.
separator, operating at said ambient or lower temperature and said ambient or lower pressure and capable of performing the processes of separating SOP from liquid, retaining and accumulating cakes of primary SOP, and concomitantly expelling liquid here designated as primary waste solution from said SOP separator. Said process of separating SOP from liquid, retaining and accumulating said cakes of primary SOP, and concomitantly expelling said primary waste solution requires use in said SOP separator of a filter and backing support, this filter and backing support here designated as SOP
filter. Said SOP
filter must be cellulose based and must not retain particles smaller than 1.0 um.
Said controlled flow rate of said dispersed primary suspension from said SOP-forming tank into said SOP separator is adjusted to be equal to or less than that of the outflow rate from said SOP separator of said primary waste solution. Said controlled flow rate is to ensure that said dispersed primary suspension within said conduit(s) between said SOP-forming tank and said SOP separator is maintained as nearly as possible as a uniformly dispersed suspension during its inflow into said SOP separator. Said primary waste solution upon exiting said SOP separator is transferred within conduit(s), using pumps and valves as necessary, to a storage tank in support of its subsequent distillation, said distillation being to recover said aliphatic alcohol.
Said SOP separator has inlet(s) that may be opened or closed and outlet(s) that may be opened or closed to permit said dispersed primary suspension or other liquid to enter and exit, respectively and, if of the centrifuge type, said SOP separator must be able to generate centripetal forces between 0 X g and 500 X g. The processes of SOP cake formation from said dispersed primary suspension followed by washing, bleaching and dehydration are specified here as they would proceed using as said SOP separator a stainless steel vertical basket centrifuge and using as said SOP filter a removable cellulosic filter bag and stainless steel wire mesh backing against a stainless steel perforated vertical basket.
It will be apparent that other devices could serve as SOP separator and other kinds of filter and backing as SOP filter, and the intention here is not to limit innovation in this realm of said basic SOP process. There are many kinds of centrifuges and centrifuge filters used in chemical, pharmaceutical, food and textile industries which are candidates for said SOP
separator used in said basic SOP process. Alternatively, a positive pressure combined filtration cake-drying system, a vacuum filtration system, a gravity-flow filtration system, or even a suitably modified clothes washing machine fitted with said SOP filter could serve as said SOP separator.
Insoluble substances within said dispersed primary suspension are accumulated as a cake of primary SOP within the bounds delimited by said SOP filter within said vertical basket while clear liquid constituting said primary waste solution concomitantly passes through said SOP filter and exits said SOP separator operating at said ambient or lower temperature and conditions of pressure intrinsic to said SOP filter and said SOP
separator. The rate at which said SOP cake number one accumulates and said primary waste solution exits is regulated by changing the angular velocity of said vertical basket such that it provides a constant centripetal force selected from within the range of 1 X g to 500 X g.
The precise operating temperature and the precise said constant centripetal force of said SOP separator may be modified in order to optimize the productivity of said basic SOP
process in relation to the species of raw plant tissue and the conditions and equipment available.
Accumulation of a cake of primary SOP within said vertical basket providing said constant centripetal force continues until the volume of said cake of primary SOP
within said SOP
It will be apparent that other devices could serve as SOP separator and other kinds of filter and backing as SOP filter, and the intention here is not to limit innovation in this realm of said basic SOP process. There are many kinds of centrifuges and centrifuge filters used in chemical, pharmaceutical, food and textile industries which are candidates for said SOP
separator used in said basic SOP process. Alternatively, a positive pressure combined filtration cake-drying system, a vacuum filtration system, a gravity-flow filtration system, or even a suitably modified clothes washing machine fitted with said SOP filter could serve as said SOP separator.
Insoluble substances within said dispersed primary suspension are accumulated as a cake of primary SOP within the bounds delimited by said SOP filter within said vertical basket while clear liquid constituting said primary waste solution concomitantly passes through said SOP filter and exits said SOP separator operating at said ambient or lower temperature and conditions of pressure intrinsic to said SOP filter and said SOP
separator. The rate at which said SOP cake number one accumulates and said primary waste solution exits is regulated by changing the angular velocity of said vertical basket such that it provides a constant centripetal force selected from within the range of 1 X g to 500 X g.
The precise operating temperature and the precise said constant centripetal force of said SOP separator may be modified in order to optimize the productivity of said basic SOP
process in relation to the species of raw plant tissue and the conditions and equipment available.
Accumulation of a cake of primary SOP within said vertical basket providing said constant centripetal force continues until the volume of said cake of primary SOP
within said SOP
filter is 50% or less of the volumetric capacity of said vertical basket, whereupon outflow of said primary dispersed suspension from said SOP-forming tank is stopped. Said vertical basket providing said constant centripetal force continues accumulating said cake of primary SOP until the volume of said primary dispersed suspension remaining in said conduit(s) between said SOP-forming tank and said SOP separator has been drained and washed from within said conduit(s) into said SOP separator, thus producing clean conduit(s). After draining said conduit(s) of said primary dispersed suspension, said clean conduit(s) is produced by introducing into said conduit(s) at its point of departure from said SOP-forming tank primary washing solution comprising 1:1 (v/v) mixture of water and said aliphatic alcohol in sufficient volume to clean said conduit(s) of said primary dispersed suspension, allowing said primary washing solution to flow into and out of said SOP
separator, using pumps as necessary. The moment said clean conduit(s) has been produced, the rate of spinning of said vertical basket is decelerated to angular velocity equal to zero.
Said cake of primary SOP is converted into bleached SOP here designated as bleached primary SOP by bleaching said cake of primary SOP contained within said vertical basket within said SOP separator for a bleaching time, here designated as primary bleaching time, selected from the range 0.2 - 1.0 hour at said ambient or lower temperature and said ambient pressure. Immediately prior to the start of said primary bleaching time, said outlet of said SOP separator is closed and bleaching solution, here designated as primary bleaching solution and comprising by volume a percentage of hydrogen peroxide selected from the range 3 - 10%, 50% 5% by volume said aliphatic alcohol and the balance water, is introduced at said ambient temperature into said vertical basket in sufficient volume to fill said SOP separator to its operational capacity. Within said range 3 - 10%, the combined volume percentages of said hydrogen peroxide and said water in said primary bleaching solution must add to 50% 5% of the total volume of said primary bleaching solution. The precise duration of said primary bleaching time and the precise percentages of said hydrogen peroxide and water within said primary bleaching solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP
process in relation to the species of raw plant tissue and the conditions and equipment available.
separator, using pumps as necessary. The moment said clean conduit(s) has been produced, the rate of spinning of said vertical basket is decelerated to angular velocity equal to zero.
Said cake of primary SOP is converted into bleached SOP here designated as bleached primary SOP by bleaching said cake of primary SOP contained within said vertical basket within said SOP separator for a bleaching time, here designated as primary bleaching time, selected from the range 0.2 - 1.0 hour at said ambient or lower temperature and said ambient pressure. Immediately prior to the start of said primary bleaching time, said outlet of said SOP separator is closed and bleaching solution, here designated as primary bleaching solution and comprising by volume a percentage of hydrogen peroxide selected from the range 3 - 10%, 50% 5% by volume said aliphatic alcohol and the balance water, is introduced at said ambient temperature into said vertical basket in sufficient volume to fill said SOP separator to its operational capacity. Within said range 3 - 10%, the combined volume percentages of said hydrogen peroxide and said water in said primary bleaching solution must add to 50% 5% of the total volume of said primary bleaching solution. The precise duration of said primary bleaching time and the precise percentages of said hydrogen peroxide and water within said primary bleaching solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP
process in relation to the species of raw plant tissue and the conditions and equipment available.
After elapse of said primary bleaching time, said outlet of said SOP separator is opened and expelling of used said primary bleaching solution, here designated as used primary bleaching solution, is begun. During the process of said expelling of said used primary bleaching solution, the angular velocity of said vertical basket is accelerated to a constant centripetal force, selected from within the range of 1 X g to 500 X g, continuing to expel said used primary bleaching solution from said SOP separator while the angular velocity of said vertical basket increases and thereafter for five additional minutes of operation of said vertical basket providing said constant centripetal force, thus achieving the goal of producing said bleached primary SOP. Said used primary bleaching solution as expelled from said SOP separator is conveyed within conduit(s), using pumps and valves as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. The precise centripetal force of said constant centripetal force used to expel said used primary bleaching solution from said SOP
separator is a variable which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached primary SOP spinning within said vertical basket providing said constant centripetal force is rinsed for a rinsing time selected from the range five to thirty minutes using a continuous spray of rinsing solution here designated as primary rinsing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol, used said primary rinsing solution here designated as used primary rinsing solution being expelled from said SOP
separator throughout said rinsing time and conveyed from there within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said primary rinsing solution has a temperature lower than said ambient temperature, and the flow rate of incoming said primary rinsing solution is the same or lower than the flow rate of outgoing said used primary rinsing solution. The precise duration of said rinsing time, the precise temperature of said primary rinsing solution and the precise flow rate of incoming said primary rinsing solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached primary SOP spinning within said vertical basket providing said constant centripetal force is converted into partially dehydrated SOP, here designated as bleached dehydrated primary SOP, by treating said bleached primary SOP with said aliphatic alcohol containing 5% or less water content, here designated as dehydration alcohol.
Said bleached primary SOP spinning in said vertical basket providing said constant centripetal force is sprayed for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol and, at the moment of spraying, having a temperature lower than said flash point. The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said dehydration alcohol, here designated as used dehydration alcohol, that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. Following completion of said spraying, said bleached primary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP
separator and from there via conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said bleached dehydrated primary SOP and said SOP filter are removed from said SOP
separator for storage or further processing as desired.
Said bleaching of said cake of primary SOP may be useful in relation to the intended end product but is non-essential for SOP production per se. When it is elected not to do said bleaching, said cake of primary SOP contained in said SOP filter within said vertical basket of said SOP separator is converted directly into washed primary SOP by washing said cake of primary SOP at said ambient or lower temperature and said ambient or lower pressure with washing solution, here designated as primary washing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol for a primary washing time selected from the range 0.2 - 1.0 hour. The precise temperature of said ambient or lower temperature, the precise pressure of said ambient or lower pressure, and the precise duration of said primary washing time are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. To initiate said washing, the outflow valve of said SOP
separator is closed, and said primary washing solution at said ambient or lower temperature is introduced into said SOP separator in sufficient volume to fill said SOP
separator to its operational capacity. Once filled to said operational capacity, the outlet of said SOP
separator is opened, and expelling of used said primary washing solution, here designated as used primary washing solution, is begun. After start of said expelling of said used primary washing solution, the angular velocity of said vertical basket is accelerated until said vertical basket provides a constant centripetal force selected from within the range of 1 X g to 500 X g, continuing to expel said used primary washing solution throughout the acceleration period and for five additional minutes after said constant centripetal force has been achieved. The precise said constant centripetal force used after said start of said expelling of said used primary washing solution may be modified in order to optimize the productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said five additional minutes, said cake of primary SOP in said vertical basket providing said constant centripetal force is subjected for the remainder of said primary washing time to a continuous spray of said primary washing solution to generate washed primary SOP and used primary washing solution, expelling throughout that time from said SOP separator said used primary washing solution. Said used primary washing solution is conveyed after said expelling within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol.
separator is a variable which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached primary SOP spinning within said vertical basket providing said constant centripetal force is rinsed for a rinsing time selected from the range five to thirty minutes using a continuous spray of rinsing solution here designated as primary rinsing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol, used said primary rinsing solution here designated as used primary rinsing solution being expelled from said SOP
separator throughout said rinsing time and conveyed from there within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said primary rinsing solution has a temperature lower than said ambient temperature, and the flow rate of incoming said primary rinsing solution is the same or lower than the flow rate of outgoing said used primary rinsing solution. The precise duration of said rinsing time, the precise temperature of said primary rinsing solution and the precise flow rate of incoming said primary rinsing solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached primary SOP spinning within said vertical basket providing said constant centripetal force is converted into partially dehydrated SOP, here designated as bleached dehydrated primary SOP, by treating said bleached primary SOP with said aliphatic alcohol containing 5% or less water content, here designated as dehydration alcohol.
Said bleached primary SOP spinning in said vertical basket providing said constant centripetal force is sprayed for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol and, at the moment of spraying, having a temperature lower than said flash point. The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said dehydration alcohol, here designated as used dehydration alcohol, that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. Following completion of said spraying, said bleached primary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP
separator and from there via conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said bleached dehydrated primary SOP and said SOP filter are removed from said SOP
separator for storage or further processing as desired.
Said bleaching of said cake of primary SOP may be useful in relation to the intended end product but is non-essential for SOP production per se. When it is elected not to do said bleaching, said cake of primary SOP contained in said SOP filter within said vertical basket of said SOP separator is converted directly into washed primary SOP by washing said cake of primary SOP at said ambient or lower temperature and said ambient or lower pressure with washing solution, here designated as primary washing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol for a primary washing time selected from the range 0.2 - 1.0 hour. The precise temperature of said ambient or lower temperature, the precise pressure of said ambient or lower pressure, and the precise duration of said primary washing time are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. To initiate said washing, the outflow valve of said SOP
separator is closed, and said primary washing solution at said ambient or lower temperature is introduced into said SOP separator in sufficient volume to fill said SOP
separator to its operational capacity. Once filled to said operational capacity, the outlet of said SOP
separator is opened, and expelling of used said primary washing solution, here designated as used primary washing solution, is begun. After start of said expelling of said used primary washing solution, the angular velocity of said vertical basket is accelerated until said vertical basket provides a constant centripetal force selected from within the range of 1 X g to 500 X g, continuing to expel said used primary washing solution throughout the acceleration period and for five additional minutes after said constant centripetal force has been achieved. The precise said constant centripetal force used after said start of said expelling of said used primary washing solution may be modified in order to optimize the productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said five additional minutes, said cake of primary SOP in said vertical basket providing said constant centripetal force is subjected for the remainder of said primary washing time to a continuous spray of said primary washing solution to generate washed primary SOP and used primary washing solution, expelling throughout that time from said SOP separator said used primary washing solution. Said used primary washing solution is conveyed after said expelling within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol.
Said washed primary SOP is converted into partially dehydrated primary SOP, here designated as dehydrated primary SOP, by spraying said washed primary SOP in said vertical basket providing said constant centripetal force for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol. The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said used dehydration alcohol that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. Following completion of said spraying, said washed primary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP separator within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said dehydrated primary SOP and said SOP filter are removed from said SOP
separator for storage or further processing as desired.
Following transfer of said entire volume of said dispersed primary suspension from said SOP-forming tank to said SOP separator during production of said cakes of primary SOP, the walls of said SOP-forming tank are washed to produce clean SOP-forming tank. Said clean SOP-forming tank is produced by washing the walls of said SOP-forming tank with said primary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed primary suspension from said SOP-forming tank to said SOP
separator.
While washing said walls of said SOP-forming tank, said primary washing solution is expelled from said SOP-forming tank via said outlet ports of said SOP-forming tank into said non-valved conduit(s) and transferred through said non-valved conduit(s) to and through said inlet(s) into said SOP separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary. After said washing of said walls of said SOP-forming tank with said primary washing solution and expelling of said primary washing solution from said SOP-forming tank, cleaning of said non-valved conduit(s) between said SOP-forming tank and said SOP separator is done. Said cleaning is accomplished by introducing into said SOP-forming tank and said outlet ports of said SOP-forming tank said primary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed primary suspension from said SOP-forming tank to said SOP
separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary.
After completion of said cleaning, said non-valved conduit(s) between said SOP-forming tank and said SOP separator is disconnected from said inlet(s) leading into said SOP
separator, and flushing of said SOP-forming tank and said non-valved conduit(s) is done.
Said flushing is accomplished by introducing into said SOP-forming tank liquid water having a temperature below the boiling point for outflow of said liquid water through said outlet ports of said SOP-forming tank hence through said non-valved conduit(s). Said flushing is continued until clear water flows freely from the disconnected end(s) of said non-valved conduit(s).
Following removal of said primary soaking solution from said extraction vessel to said SOP-forming tank for production of said primary suspension, said insoluble residue remaining in said extraction vessel is subjected for a time to a second soak by fully immersing said insoluble residue in a secondary soaking solution at said ambient temperature and said ambient pressure to yield a second extract for conveyance to and production within said SOP-forming tank or its equivalent of a secondary suspension for processing into additional cakes of SOP here designated as cakes of secondary SOP. Said secondary soaking solution consists of a known concentration, ranging from 0.5 - 10 M, of an alkaline hydroxide in aqueous solution. The species of said alkaline hydroxide may be lithium hydroxide, potassium hydroxide or sodium hydroxide. Said secondary soaking solution is provided to said extraction vessel in sufficient or greater volume needed to achieve a soak, here designated as secondary soak, of all said insoluble residue in said extraction vessel for the full duration of secondary soaking time selected from within the range 0.1 -4.0 hours at a temperature selected from within the range 4 - 100 C. The species and concentration of said alkaline hydroxide, the precise duration of said secondary soaking time, and the precise temperature(s) of said secondary soaking solution used during said secondary soaking time are, within the stated bounds, variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said secondary soaking time, said secondary soaking solution is displaced from said insoluble residue remaining in said extraction vessel using gravity flow, positive pressure or vacuum expulsion to expel the recoverable volume of said secondary soaking solution, here designated as secondary recoverable volume, into conduit(s) running from said extraction vessel to said SOP-forming tank. Said secondary recoverable volume is transferred within said conduit(s) from said extraction vessel into said SOP-forming tank using valves and pumps as necessary. Said secondary recoverable volume is retained in said SOP-forming tank until the temperature of the liquid of said secondary recoverable volume is measured to be at or below said ambient temperature.
Following removal from said extraction vessel of said secondary recoverable volume, said insoluble residue remaining in said extraction vessel is further processed in whatever way desired, an obvious way being to carry said insoluble residue through the usual pulping process in support of subsequent production of paper and related cellulosic products. If disposal into the environment is opted for, an important consideration is that said insoluble residue is enriched in alkaline hydroxide content and therefore would be potentially harmful to life if it were not first neutralized and desalted by some means.
An aliphatic alcohol in liquid state of at least 95% purity, containing by volume 5% or less water, and pre-chilled to a temperature at least 10 0C below its flash point is transferred within conduit(s), using valves and pumps as necessary, from an alcohol storage tank into said SOP-forming tank containing said secondary recoverable volume. Suitable species of said aliphatic alcohol include ethanol, methanol, 2-propanol or n-butanol.
Said aliphatic alcohol is added to said secondary recoverable volume until the total volume of liquid contained in said SOP-forming tank is twice, within volumetric precision of 2%, that of said secondary recoverable volume. Said total volume of liquid contained in said SOP-forming tank is mixed for a time, here designated as secondary mixing time, selected from the range 1 - 30 minutes, the duration of said secondary mixing time being sufficient to achieve uniform mixing thus producing a 1:1 (v/ v) homogeneous mixture, here designated as secondary mixture, of said secondary recoverable volume and the equivalent volume of said aliphatic alcohol. Following elapse of said secondary mixing time, said secondary mixture is held static at said ambient temperature and said ambient pressure in said SOP-forming tank for a setting time, here designated as secondary setting time, selected from the range 0.1 - 24 hours. During the course of said secondary setting time, a fluid suspension of coagulated substances containing oligosaccharides and polysaccharides, and here designated as secondary suspension, forms. The species of said aliphatic alcohol, the precise duration of said secondary mixing time and the precise duration of said secondary setting time are, within the stated bounds, variables which may be modified in order to optimize the productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
After elapse of said secondary setting time, said secondary suspension in said SOP-forming tank is stirred or mixed continuously for a time, here designated as secondary stirring time, at said ambient temperature and said ambient pressure to produce a dispersed secondary suspension. Said secondary stirring time is whatever length of time is required to transfer the entire volume of said dispersed secondary suspension generated from said secondary recoverable volume and the equivalent volume of added said aliphatic alcohol out of said SOP-forming tank, conveying it using pumps as necessary from said SOP-forming tank at a controlled flow rate within non-valved conduit(s) to said SOP separator operating at said ambient or lower temperature and said ambient or lower pressure and capable of performing the processes of separating SOP from liquid, retaining and accumulating said cakes of secondary SOP, and concomitantly expelling liquid here designated as secondary waste solution from said SOP separator. Said process of separating SOP from liquid, retaining and accumulating said cakes of secondary SOP, and concomitantly expelling said secondary waste solution requires use in said SOP separator of said SOP
filter. Said SOP
filter must be cellulose based and must not retain particles smaller than 1.0 pm.
Said controlled flow rate of said dispersed secondary suspension from said SOP-forming tank into said SOP separator is adjusted to be equal to or less than that of the outflow rate from said SOP separator of said secondary waste solution. Said controlled flow rate is to ensure that said dispersed secondary suspension within said conduit(s) between said SOP-forming tank and said SOP separator is maintained as nearly as possible as a uniformly dispersed suspension during its inflow into said SOP separator. Said secondary waste solution upon exiting said SOP separator is transferred within conduit(s), using pumps and valves as necessary, to a storage tank in support of its subsequent distillation, said distillation being to recover said aliphatic alcohol.
Said SOP separator has inlet(s) that may be opened or closed and outlet(s) that may be opened or closed to permit said dispersed secondary suspension or other liquid to enter and exit, respectively and, if of the centrifuge type, said SOP separator must be able to generate centripetal forces between 0 X g and 500 X g. The processes of SOP cake formation from said dispersed secondary suspension followed by¨washing, bleaching and dehydration are specified here as they would proceed using as said SOP separator a stainless steel vertical basket centrifuge and using as said SOP filter a removable cellulosic filter bag and stainless steel wire mesh backing against a stainless steel perforated vertical basket.
It will be apparent that other devices could serve as SOP separator and other kinds of filter and backing as SOP filter, and the intention here is not to limit innovation in this realm of said basic SOP process. There are many kinds of centrifuges and centrifuge filters used in chemical, pharmaceutical, food and textile industries which are candidates for said SOP
separator used in said basic SOP process. Alternatively, a positive pressure combined filtration cake-drying system, a vacuum filtration system, a gravity-flow filtration system, or even a suitably modified clothes washing machine fitted with said SOP filter could serve as said SOP separator.
Insoluble substances within said dispersed secondary suspension are accumulated as a cake, here designated as a cake of secondary SOP within the bounds delimited by said SOP filter within said vertical basket while clear liquid, here designated as secondary waste solution, concomitantly passes through said SOP filter and exits said SOP separator operating at said ambient or lower lemperature and conditions of pressure intrinsic to said SOP
filter and said SOP separator. During accumulation of said cake of secondary SOP within said vertical basket of said SOP separator, said controlled flow rate of said dispersed secondary suspension from said SOP-forming tank into said SOP separator is adjusted to be equal to or less than that of the outflow rate from said SOP separator of said secondary waste solution.
Said controlled flow rate is to ensure that said dispersed secondary suspension within the conduit(s) between said SOP-forming tank and said SOP separator is maintained as nearly as possible as a uniformly dispersed suspension during its inflow into said SOP separator.
Said secondary waste solution upon exiting said SOP separator is transferred within conduit(s), using valves and pumps and necessary, to a storage tank in support of its subsequent distillation, said distillation being to recover said aliphatic alcohol. The rate at which said cake of secondary SOP accumulates and said secondary waste solution exits is regulated by changing the angular velocity of said vertical basket such that it provides a constant centripetal force selected from within the range of 1 X g to 500 X g.
Accumulation of said cake of secondary SOP within said vertical basket providing said constant centripetal force continues until the volume of said cake of secondary SOP within said SOP
filter is 50%
or less of the volumetric capacity of said vertical basket, whereupon outflow of said secondary dispersed suspension from said SOP-forming tank is stopped. Said vertical basket providing said constant centripetal force continues accumulating said cake of secondary SOP until the volume of said secondary dispersed suspension remaining in said SOP-forming tank and said conduit(s) between said SOP-forming tank and said SOP
separator has been drained and washed from within said conduit(s) into said SOP separator, thus producing clean conduit(s). After draining said conduit(s) of said secondary dispersed suspension, said clean conduit(s) is produced by introducing into said conduit(s) at its point of departure from said SOP-forming tank said secondary washing solution comprising 1:1 (v/ v) mixture of water and said aliphatic in sufficient volume to clean said conduit(s) of said secondary dispersed suspension, allowing said secondary washing solution to flow into and out of said SOP separator, using pumps as necessary. The moment said clean conduit has been produced, the rate of spinning of said vertical basket is decelerated to angular velocity equal to zero.
Said cake of secondary SOP is converted into bleached SOP here designated as bleached secondary SOP by bleaching said cake of secondary SOP contained within said vertical basket within said SOP separator for a bleaching time, here designated as secondary bleaching time, selected from the range 0.2 - 1.0 hour at said ambient or lower temperature and said ambient pressure. Immediately prior to the start of said secondary bleaching time, said outlet of said SOP separator is closed and bleaching solution, here designated as secondary bleaching solution and comprising by volume a percentage of hydrogen peroxide selected from the range 3 - 10%, 50% 5% by volume said aliphatic alcohol and the balance water, is introduced at said ambient temperature into said vertical basket in sufficient volume to fill said SOP separator to its operational capacity. Within said range 3 - 10%, the combined volume percentages of said hydrogen peroxide and said water in said secondary bleaching solution must add to 50% 5% of the total volume of said secondary bleaching solution. The precise duration of said secondary bleaching time and the precise percentages of said hydrogen peroxide and water within said secondary bleaching solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
After expiry of said secondary bleaching time, said outlet of said SOP
separator is opened and expelling of used said secondary bleaching solution, here designated as used secondary bleaching solution, is begun. During the process of said expelling of said used secondary bleaching solution, the angular velocity of said vertical basket is accelerated to a constant centripetal force, selected from within the range of 1 X g to 500 X g, continuing to expel said used secondary bleaching solution from said SOP separator while the angular velocity of said vertical basket increases and thereafter for five additional minutes of operation of said vertical basket providing said constant centripetal force, thus achieving the goal of producing said bleached secondary SOP. Said used secondary bleaching solution as expelled from said SOP separator is conveyed within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. The precise centripetal force of said constant centripetal force used to expel said used secondary bleaching solution from said SOP separator is a variable which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached secondary SOP spinning within said vertical basket providing said constant centripetal force is rinsed for a rinsing time selected from the range five to thirty minutes using a continuous spray of rinsing solution here designated as secondary rinsing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol, used said secondary rinsing solution here designated as used secondary rinsing solution being expelled from said SOP separator throughout said rinsing time and conveyed from there within conduit(s), using valves and pumps as necessary, to a suitable storage tafflc in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said secondary rinsing solution has a temperature lower than said ambient temperature, and the flow rate of incoming said secondary rinsing solution is the same or lower than the flow rate of outgoing said used secondary rinsing solution. The precise duration of said rinsing time, the precise temperature of said secondary rinsing solution and the precise flow rate of incoming said secondary rinsing solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached secondary SOP spinning within said vertical basket providing said constant centripetal force is converted into partially dehydrated SOP, here designated as bleached dehydrated secondary SOP, by treating said bleached secondary SOP with said dehydration alcohol. Said bleached secondary SOP spinning in said vertical basket providing said constant centripetal force is sprayed for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol and, at the moment of spraying, having a temperature lower than said flash point.
The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said dehydration alcohol that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following completion of said spraying, said bleached secondary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP separator and from there via conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said bleached dehydrated secondary SOP and said SOP filter are removed from said SOP separator for storage or further processing as desired.
Said bleaching of said cake of secondary SOP may be useful in relation to the intended end product but is non-essential for SOP production per se. When it is elected not to do said bleaching, said cake of secondary SOP contained in said SOP filter within said vertical basket of said SOP separator is converted directly into washed secondary SOP
by washing said cake of secondary SOP cake at said ambient or lower temperature and said ambient or lower pressure with washing solution, here designated as secondary washing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol for a secondary washing time selected from the range 0.2 - 1.0 hour. The precise temperature of said ambient or lower temperature, the precise pressure of said ambient or lower pressure, and the precise duration of said secondary washing time are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. To initiate said washing, the outflow valve of said SOP separator is closed, and said secondary washing solution at said ambient or lower temperature is introduced into said SOP separator in sufficient volume to fill said SOP separator to its operational capacity. Once filled to said operational capacity, the outlet of said SOP separator is opened, and expelling of used said secondary washing solution, here designated as used secondary washing solution, is begun. After start of said expelling of said used secondary washing solution, the angular velocity of said vertical basket is accelerated until said vertical basket provides a constant centripetal force selected from within the range of 1 X g to 500 X g, continuing to expel said used secondary washing solution throughout the acceleration period and for five additional minutes after said constant centripetal force has been achieved. The precise said constant centripetal force used after said start of said expelling of said used secondary washing solution may be modified in order to optimize the productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said five additional minutes, said cake of secondary SOP
in said vertical basket providing said constant centripetal force is subjected for the remainder of said secondary washing time to a continuous spray of said secondary washing solution to generate washed secondary SOP and used secondary washing solution, expelling throughout that time from said SOP separator said used secondary washing solution. Said used secondary washing solution is conveyed after said expelling within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol.
Said washed secondary SOP is converted into partially dehydrated secondary SOP, here designated as dehydrated secondary SOP, by spraying said washed secondary SOP
in said vertical basket providing said constant centripetal force for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol. The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said used dehydration alcohol that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. Following completion of said spraying, said washed secondary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP separator within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said dehydrated secondary SOP and said SOP filter are removed from said SOP separator for storage or further processing as desired.
Following transfer of said entire volume of said dispersed secondary suspension from said SOP-forming tank to said SOP separator during production of said cakes of secondary SOP, the walls of said SOP-forming tank are washed to produce clean SOP-forming tank. Said clean SOP-forming tank is produced by washing the walls of said SOP-forming tank with said secondary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed secondary suspension from said SOP-forming tank to said SOP
separator. While washing said walls of said SOP-forming tank, said secondary washing solution is expelled from said SOP-forming tank via said outlet ports of said SOP-forming tank into said non-valved conduit(s) and transferred through said non-valved conduit(s) to and through said inlet(s) into said SOP separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary. After said washing of said walls of said SOP-forming tank with said secondary washing solution and expelling of said secondary washing solution from said SOP-forming tank, cleaning of said non-valved conduit(s) between said SOP-forming tank and said SOP separator is done. Said cleaning is accomplished by introducing into said SOP-forming tank and said outlet ports of said SOP-forming tank said secondary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed secondary suspension from said SOP-forming tank to said SOP separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary.
After completion of said cleaning, said non-valved conduit(s) between said SOP-forming tank and said SOP separator is disconnected from said inlet(s) leading into said SOP
separator, and flushing of said SOP-forming tank and said non-valved conduit(s) is done.
Said flushing is accomplished by introducing into said SOP-forming tank liquid water having a temperature below the boiling point for outflow of said liquid water through said outlet ports of said SOP-forming tank hence through said non-valved conduit(s). Said flushing is continued until clear water flows freely from the disconnected end(s) of said non-valved conduit(s).
Cakes of SOP, whether of primary or secondary designation, bleached or unbleached, hydrated or partially dehydrated, as produced in said basic SOP process are miscible in water upon stirring. A
clear solution of water miscible oligosaccharides and polysaccharides, here designated as MOP, is produced by weighing a mass of said SOP and adding to said mass a volume in litres of water equaling at least twice the mass in kilograms of said SOP, followed by stirring the mixture at said ambient pressure and a temperature between 0 oC and 100 oC until a clear solution is obtained. The precise temperature of said stirring to produce said MOP is a variable which may be modified in order to optimize the efficiency and productivity of the process in relation to the species of raw plant tissue and the conditions and equipment available. Said MOP is a convenient way to transport and further refine SOP.
Said distillation is specified as part of the overall said basic SOP process, and said distillation is done in a distillation apparatus in order to recover and, if so desired, to recycle said aliphatic alcohol. Said distillation is not essential for production of SOP
using said basic SOP process, but said distillation serves to prevent the environmental contamination which might otherwise occur, and said distillation also presents the opportunity for the aqueous residue remaining after said distillation also to be used again. Recovery by volume of said aliphatic alcohol during said distillation is in the range of 85 - 95% of the volumes of said aliphatic alcohol introduced into said SOP forming tank to produce said primary suspension and said secondary suspension. If said distillation employs boiling at ambient pressure at or near the boiling temperature of said aliphatic alcohol, said aliphatic alcohol is recovered in marginally higher yield than if said distillation employs vacuum distillation at a temperature below the ambient boiling temperature.
Said aqueous residue remaining after said distillation can be transferred via conduit(s), using pumps and valves as necessary, from said distillation apparatus to fill an alkali storage tank to a known volume. Said alkali storage tank must be capable of stirring and/or mixing its contents at said ambient temperature and pressure. Said aqueous residue transferred from said distillation apparatus into said alkali storage tank is titrated for its alkaline hydroxide content followed by addition to said aqueous residue sufficient amount of said alkaline hydroxide to produce alkaline soaking solution that fulfils the specified requirement of said known concentration of said primary soaking solution or said secondary soaking solution. From said alkali storage tank, said alkaline soaking solution is transferred to said extraction vessel to achieve a said primary soak or a said secondary soak of another batch of said pieces of raw plant tissue of dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length. In this way, said aqueous residue can be recycled through said basic SOP process.
Following repeated recycling of said aqueous residue in support of the production of successive batches of SOP using said basic SOP process, an insoluble precipitate forms in said aqueous residue within said distillation apparatus during or after said distillation. Said insoluble precipitate is formed from substances which were extracted from said pieces of raw plant tissue and/or from said insoluble residue of said pieces of raw plant tissue during said primary soak and/or said secondary soak, respectively. Said insoluble precipitate comprises chemical substances potentially of high economic value and, following removal from said distillation apparatus of the clear liquid component of said aqueous residue, said insoluble precipitate remaining in said distillation apparatus may be recovered either by physical means or by dissolving said insoluble precipitate in an appropriate solvent and removing that solution, simultaneously cleaning said distillation unit. Said clear liquid component of said aqueous residue is transferred via conduit(s), using pumps and valves as necessary, from said distillation apparatus to fill to a known volume said alkali storage tank capable of stirring and/or mixing its contents at ambient temperature and pressure. Said clear liquid component of said aqueous residue transferred from said distillation apparatus into said alkali storage tank is titrated for its alkaline hydroxide content followed by addition to said aqueous residue sufficient amount of said alkaline hydroxide to produce alkaline soaking solution that fulfils the specified requirement of said known concentration of said primary soaking solution or said secondary soaking solution. From said alkali storage tank, said alkaline soaking solution is transferred to said extraction vessel to achieve a said primary soak or a said secondary soak of another batch of said pieces of raw plant tissue of dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length.
If disposal into the environment rather than recycling of said aqueous residue is opted for, it deserves emphasis that said aqueous residue is enriched in alkaline hydroxide content and therefore is potentially harmful to life if not first neutralized and desalted by some means, for example, by addition of acid to lower the pH and enable removal of the high salt concentration.
A number of variables potentially affecting SOP yield and/or cost are listed below in relation to production of said number one bleached dehydrated SOP, only, but this listing also serves to reveal the broad methodological versatility available to said basic SOP process in relation to production of SOP in general. A non-comprehensive list of said variables includes the following:
1) said plant species which is processed;
2) anatomical and chemical composition including water content of said raw pieces of plant tissue processed;
3) kind and size of said extraction vessel used;
4) alkaline hydroxide metal(s), viz., sodium potassium, lithium, selected for use in said primary soaking solution;
5) said known concentration of said alkaline hydroxide used in said primary soaking solution;
6) duration of said primary soaking time in said extraction vessel;
7) temperature of said primary soaking solution in said extraction vessel;
8) method used to displace and transfer said primary soaking solution from said extraction vessel to said SOP-forming tank;
9) respecting said conduit(s) between said extraction vessel and said SOP-forming tank, said conduit(s) between said SOP-forming tank and said SOP separator, and said conduit(s) between said SOP separator and tanks receiving solutions expelled from said SOP separator, all must be compatible with said alkaline hydroxide and said aliphatic alcohol and, therefore, it is recommended that all be of inert plastic;
however, shape, wall thickness, and dimensions of said conduit(s) are not specified here;
10) non-specified features of said SOP forming tank;
11) kind of said aliphatic alcohol added to said SOP forming tank to produce said primary suspension;
12) duration of said mixing time in said SOP forming tank to produce said primary mixture;
13) method and intensity of mixing to achieve said primary mixture in said SOP
forming tank;
14) duration of said setting time to produce said primary suspension;
15) nature of said SOP separator and said SOP filter;
16) physical environment setpoints used during separation of SOP batch number one from the 1:1 (v/v) mixture of alkaline soaking solution and aliphatic alcohol;
17) duration of washing, bleaching, rinsing and dehydrating the SOP cake.
Example Data arising from application of said basic SOP process to pieces of wood from Betula populifolia are presented herewith in Figure 1 and Tables 1-11, and data on SOP yields from tissues of a number of additional plant species using said basic SOP process are also presented in Tables 11 and 12. However, said data are not to specify that said basic SOP
process as stated for B. populifolia and said additional plant species must be rigidly adhered to for either those or other plant species. Using said basic SOP process, some quantity of SOP evidently can be obtained from any tissue of any plant species, and the methodological latitude within said basic SOP process invites modifications in order to increase SOP yield and reduce costs.
The chemistry of SOP from Betula populifolia wood was investigated in some depth, by dialysis followed by sulfuric acid hydrolysis of the SOP followed by barium carbonate neutralization, drying, trimethylsilylation and analysis by combined gas chromatography -mass spectroscopy (GC/ MS). Dialysis through cellulose acetate of different molecular-weight cutoffs established that B. populifolia SOP comprises a small fraction of short-chain oligosaccharides as well as larger polysaccharides, the major fraction being above 10,000 Daltons. GC/MS analysis of hydrolyzed, trimethylsilylated SOP revealed that B.
populifolia SOP contains equal amounts of D-xylose and 4-mefftylglucuronic acid as its dominant building blocks. Those two compounds are well known constituents of Magnoliophyta hemicelluloses, and thus said basic SOP process is a simple and rapid method to mass produce those two compounds. However, considerable research remains to be done in order to understand the chemistry of SOP as it may vary among plant species.
Data on SOP production from wood of Betula populifolia using the basic SOP
process.
Figure 1. Percentage yield of SOP from dry, raw wood of Betula populifolia as a function of temperature and NaOH molarity.
Linear twater (control)) 4.
- - Linear OM Na011) SOP
separator for storage or further processing as desired.
Following transfer of said entire volume of said dispersed primary suspension from said SOP-forming tank to said SOP separator during production of said cakes of primary SOP, the walls of said SOP-forming tank are washed to produce clean SOP-forming tank. Said clean SOP-forming tank is produced by washing the walls of said SOP-forming tank with said primary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed primary suspension from said SOP-forming tank to said SOP
separator.
While washing said walls of said SOP-forming tank, said primary washing solution is expelled from said SOP-forming tank via said outlet ports of said SOP-forming tank into said non-valved conduit(s) and transferred through said non-valved conduit(s) to and through said inlet(s) into said SOP separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary. After said washing of said walls of said SOP-forming tank with said primary washing solution and expelling of said primary washing solution from said SOP-forming tank, cleaning of said non-valved conduit(s) between said SOP-forming tank and said SOP separator is done. Said cleaning is accomplished by introducing into said SOP-forming tank and said outlet ports of said SOP-forming tank said primary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed primary suspension from said SOP-forming tank to said SOP
separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary.
After completion of said cleaning, said non-valved conduit(s) between said SOP-forming tank and said SOP separator is disconnected from said inlet(s) leading into said SOP
separator, and flushing of said SOP-forming tank and said non-valved conduit(s) is done.
Said flushing is accomplished by introducing into said SOP-forming tank liquid water having a temperature below the boiling point for outflow of said liquid water through said outlet ports of said SOP-forming tank hence through said non-valved conduit(s). Said flushing is continued until clear water flows freely from the disconnected end(s) of said non-valved conduit(s).
Following removal of said primary soaking solution from said extraction vessel to said SOP-forming tank for production of said primary suspension, said insoluble residue remaining in said extraction vessel is subjected for a time to a second soak by fully immersing said insoluble residue in a secondary soaking solution at said ambient temperature and said ambient pressure to yield a second extract for conveyance to and production within said SOP-forming tank or its equivalent of a secondary suspension for processing into additional cakes of SOP here designated as cakes of secondary SOP. Said secondary soaking solution consists of a known concentration, ranging from 0.5 - 10 M, of an alkaline hydroxide in aqueous solution. The species of said alkaline hydroxide may be lithium hydroxide, potassium hydroxide or sodium hydroxide. Said secondary soaking solution is provided to said extraction vessel in sufficient or greater volume needed to achieve a soak, here designated as secondary soak, of all said insoluble residue in said extraction vessel for the full duration of secondary soaking time selected from within the range 0.1 -4.0 hours at a temperature selected from within the range 4 - 100 C. The species and concentration of said alkaline hydroxide, the precise duration of said secondary soaking time, and the precise temperature(s) of said secondary soaking solution used during said secondary soaking time are, within the stated bounds, variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said secondary soaking time, said secondary soaking solution is displaced from said insoluble residue remaining in said extraction vessel using gravity flow, positive pressure or vacuum expulsion to expel the recoverable volume of said secondary soaking solution, here designated as secondary recoverable volume, into conduit(s) running from said extraction vessel to said SOP-forming tank. Said secondary recoverable volume is transferred within said conduit(s) from said extraction vessel into said SOP-forming tank using valves and pumps as necessary. Said secondary recoverable volume is retained in said SOP-forming tank until the temperature of the liquid of said secondary recoverable volume is measured to be at or below said ambient temperature.
Following removal from said extraction vessel of said secondary recoverable volume, said insoluble residue remaining in said extraction vessel is further processed in whatever way desired, an obvious way being to carry said insoluble residue through the usual pulping process in support of subsequent production of paper and related cellulosic products. If disposal into the environment is opted for, an important consideration is that said insoluble residue is enriched in alkaline hydroxide content and therefore would be potentially harmful to life if it were not first neutralized and desalted by some means.
An aliphatic alcohol in liquid state of at least 95% purity, containing by volume 5% or less water, and pre-chilled to a temperature at least 10 0C below its flash point is transferred within conduit(s), using valves and pumps as necessary, from an alcohol storage tank into said SOP-forming tank containing said secondary recoverable volume. Suitable species of said aliphatic alcohol include ethanol, methanol, 2-propanol or n-butanol.
Said aliphatic alcohol is added to said secondary recoverable volume until the total volume of liquid contained in said SOP-forming tank is twice, within volumetric precision of 2%, that of said secondary recoverable volume. Said total volume of liquid contained in said SOP-forming tank is mixed for a time, here designated as secondary mixing time, selected from the range 1 - 30 minutes, the duration of said secondary mixing time being sufficient to achieve uniform mixing thus producing a 1:1 (v/ v) homogeneous mixture, here designated as secondary mixture, of said secondary recoverable volume and the equivalent volume of said aliphatic alcohol. Following elapse of said secondary mixing time, said secondary mixture is held static at said ambient temperature and said ambient pressure in said SOP-forming tank for a setting time, here designated as secondary setting time, selected from the range 0.1 - 24 hours. During the course of said secondary setting time, a fluid suspension of coagulated substances containing oligosaccharides and polysaccharides, and here designated as secondary suspension, forms. The species of said aliphatic alcohol, the precise duration of said secondary mixing time and the precise duration of said secondary setting time are, within the stated bounds, variables which may be modified in order to optimize the productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
After elapse of said secondary setting time, said secondary suspension in said SOP-forming tank is stirred or mixed continuously for a time, here designated as secondary stirring time, at said ambient temperature and said ambient pressure to produce a dispersed secondary suspension. Said secondary stirring time is whatever length of time is required to transfer the entire volume of said dispersed secondary suspension generated from said secondary recoverable volume and the equivalent volume of added said aliphatic alcohol out of said SOP-forming tank, conveying it using pumps as necessary from said SOP-forming tank at a controlled flow rate within non-valved conduit(s) to said SOP separator operating at said ambient or lower temperature and said ambient or lower pressure and capable of performing the processes of separating SOP from liquid, retaining and accumulating said cakes of secondary SOP, and concomitantly expelling liquid here designated as secondary waste solution from said SOP separator. Said process of separating SOP from liquid, retaining and accumulating said cakes of secondary SOP, and concomitantly expelling said secondary waste solution requires use in said SOP separator of said SOP
filter. Said SOP
filter must be cellulose based and must not retain particles smaller than 1.0 pm.
Said controlled flow rate of said dispersed secondary suspension from said SOP-forming tank into said SOP separator is adjusted to be equal to or less than that of the outflow rate from said SOP separator of said secondary waste solution. Said controlled flow rate is to ensure that said dispersed secondary suspension within said conduit(s) between said SOP-forming tank and said SOP separator is maintained as nearly as possible as a uniformly dispersed suspension during its inflow into said SOP separator. Said secondary waste solution upon exiting said SOP separator is transferred within conduit(s), using pumps and valves as necessary, to a storage tank in support of its subsequent distillation, said distillation being to recover said aliphatic alcohol.
Said SOP separator has inlet(s) that may be opened or closed and outlet(s) that may be opened or closed to permit said dispersed secondary suspension or other liquid to enter and exit, respectively and, if of the centrifuge type, said SOP separator must be able to generate centripetal forces between 0 X g and 500 X g. The processes of SOP cake formation from said dispersed secondary suspension followed by¨washing, bleaching and dehydration are specified here as they would proceed using as said SOP separator a stainless steel vertical basket centrifuge and using as said SOP filter a removable cellulosic filter bag and stainless steel wire mesh backing against a stainless steel perforated vertical basket.
It will be apparent that other devices could serve as SOP separator and other kinds of filter and backing as SOP filter, and the intention here is not to limit innovation in this realm of said basic SOP process. There are many kinds of centrifuges and centrifuge filters used in chemical, pharmaceutical, food and textile industries which are candidates for said SOP
separator used in said basic SOP process. Alternatively, a positive pressure combined filtration cake-drying system, a vacuum filtration system, a gravity-flow filtration system, or even a suitably modified clothes washing machine fitted with said SOP filter could serve as said SOP separator.
Insoluble substances within said dispersed secondary suspension are accumulated as a cake, here designated as a cake of secondary SOP within the bounds delimited by said SOP filter within said vertical basket while clear liquid, here designated as secondary waste solution, concomitantly passes through said SOP filter and exits said SOP separator operating at said ambient or lower lemperature and conditions of pressure intrinsic to said SOP
filter and said SOP separator. During accumulation of said cake of secondary SOP within said vertical basket of said SOP separator, said controlled flow rate of said dispersed secondary suspension from said SOP-forming tank into said SOP separator is adjusted to be equal to or less than that of the outflow rate from said SOP separator of said secondary waste solution.
Said controlled flow rate is to ensure that said dispersed secondary suspension within the conduit(s) between said SOP-forming tank and said SOP separator is maintained as nearly as possible as a uniformly dispersed suspension during its inflow into said SOP separator.
Said secondary waste solution upon exiting said SOP separator is transferred within conduit(s), using valves and pumps and necessary, to a storage tank in support of its subsequent distillation, said distillation being to recover said aliphatic alcohol. The rate at which said cake of secondary SOP accumulates and said secondary waste solution exits is regulated by changing the angular velocity of said vertical basket such that it provides a constant centripetal force selected from within the range of 1 X g to 500 X g.
Accumulation of said cake of secondary SOP within said vertical basket providing said constant centripetal force continues until the volume of said cake of secondary SOP within said SOP
filter is 50%
or less of the volumetric capacity of said vertical basket, whereupon outflow of said secondary dispersed suspension from said SOP-forming tank is stopped. Said vertical basket providing said constant centripetal force continues accumulating said cake of secondary SOP until the volume of said secondary dispersed suspension remaining in said SOP-forming tank and said conduit(s) between said SOP-forming tank and said SOP
separator has been drained and washed from within said conduit(s) into said SOP separator, thus producing clean conduit(s). After draining said conduit(s) of said secondary dispersed suspension, said clean conduit(s) is produced by introducing into said conduit(s) at its point of departure from said SOP-forming tank said secondary washing solution comprising 1:1 (v/ v) mixture of water and said aliphatic in sufficient volume to clean said conduit(s) of said secondary dispersed suspension, allowing said secondary washing solution to flow into and out of said SOP separator, using pumps as necessary. The moment said clean conduit has been produced, the rate of spinning of said vertical basket is decelerated to angular velocity equal to zero.
Said cake of secondary SOP is converted into bleached SOP here designated as bleached secondary SOP by bleaching said cake of secondary SOP contained within said vertical basket within said SOP separator for a bleaching time, here designated as secondary bleaching time, selected from the range 0.2 - 1.0 hour at said ambient or lower temperature and said ambient pressure. Immediately prior to the start of said secondary bleaching time, said outlet of said SOP separator is closed and bleaching solution, here designated as secondary bleaching solution and comprising by volume a percentage of hydrogen peroxide selected from the range 3 - 10%, 50% 5% by volume said aliphatic alcohol and the balance water, is introduced at said ambient temperature into said vertical basket in sufficient volume to fill said SOP separator to its operational capacity. Within said range 3 - 10%, the combined volume percentages of said hydrogen peroxide and said water in said secondary bleaching solution must add to 50% 5% of the total volume of said secondary bleaching solution. The precise duration of said secondary bleaching time and the precise percentages of said hydrogen peroxide and water within said secondary bleaching solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
After expiry of said secondary bleaching time, said outlet of said SOP
separator is opened and expelling of used said secondary bleaching solution, here designated as used secondary bleaching solution, is begun. During the process of said expelling of said used secondary bleaching solution, the angular velocity of said vertical basket is accelerated to a constant centripetal force, selected from within the range of 1 X g to 500 X g, continuing to expel said used secondary bleaching solution from said SOP separator while the angular velocity of said vertical basket increases and thereafter for five additional minutes of operation of said vertical basket providing said constant centripetal force, thus achieving the goal of producing said bleached secondary SOP. Said used secondary bleaching solution as expelled from said SOP separator is conveyed within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. The precise centripetal force of said constant centripetal force used to expel said used secondary bleaching solution from said SOP separator is a variable which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached secondary SOP spinning within said vertical basket providing said constant centripetal force is rinsed for a rinsing time selected from the range five to thirty minutes using a continuous spray of rinsing solution here designated as secondary rinsing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol, used said secondary rinsing solution here designated as used secondary rinsing solution being expelled from said SOP separator throughout said rinsing time and conveyed from there within conduit(s), using valves and pumps as necessary, to a suitable storage tafflc in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said secondary rinsing solution has a temperature lower than said ambient temperature, and the flow rate of incoming said secondary rinsing solution is the same or lower than the flow rate of outgoing said used secondary rinsing solution. The precise duration of said rinsing time, the precise temperature of said secondary rinsing solution and the precise flow rate of incoming said secondary rinsing solution are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Said bleached secondary SOP spinning within said vertical basket providing said constant centripetal force is converted into partially dehydrated SOP, here designated as bleached dehydrated secondary SOP, by treating said bleached secondary SOP with said dehydration alcohol. Said bleached secondary SOP spinning in said vertical basket providing said constant centripetal force is sprayed for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol and, at the moment of spraying, having a temperature lower than said flash point.
The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said dehydration alcohol that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following completion of said spraying, said bleached secondary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP separator and from there via conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said bleached dehydrated secondary SOP and said SOP filter are removed from said SOP separator for storage or further processing as desired.
Said bleaching of said cake of secondary SOP may be useful in relation to the intended end product but is non-essential for SOP production per se. When it is elected not to do said bleaching, said cake of secondary SOP contained in said SOP filter within said vertical basket of said SOP separator is converted directly into washed secondary SOP
by washing said cake of secondary SOP cake at said ambient or lower temperature and said ambient or lower pressure with washing solution, here designated as secondary washing solution and comprising 1:1 (v/v) mixture of water and said aliphatic alcohol for a secondary washing time selected from the range 0.2 - 1.0 hour. The precise temperature of said ambient or lower temperature, the precise pressure of said ambient or lower pressure, and the precise duration of said secondary washing time are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. To initiate said washing, the outflow valve of said SOP separator is closed, and said secondary washing solution at said ambient or lower temperature is introduced into said SOP separator in sufficient volume to fill said SOP separator to its operational capacity. Once filled to said operational capacity, the outlet of said SOP separator is opened, and expelling of used said secondary washing solution, here designated as used secondary washing solution, is begun. After start of said expelling of said used secondary washing solution, the angular velocity of said vertical basket is accelerated until said vertical basket provides a constant centripetal force selected from within the range of 1 X g to 500 X g, continuing to expel said used secondary washing solution throughout the acceleration period and for five additional minutes after said constant centripetal force has been achieved. The precise said constant centripetal force used after said start of said expelling of said used secondary washing solution may be modified in order to optimize the productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available.
Following elapse of said five additional minutes, said cake of secondary SOP
in said vertical basket providing said constant centripetal force is subjected for the remainder of said secondary washing time to a continuous spray of said secondary washing solution to generate washed secondary SOP and used secondary washing solution, expelling throughout that time from said SOP separator said used secondary washing solution. Said used secondary washing solution is conveyed after said expelling within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol.
Said washed secondary SOP is converted into partially dehydrated secondary SOP, here designated as dehydrated secondary SOP, by spraying said washed secondary SOP
in said vertical basket providing said constant centripetal force for five minutes with said dehydration alcohol pre-chilled to a temperature at least 10 0C below the flash point of said dehydration alcohol. The flow rate of incoming said dehydration alcohol is the same or lower than the flow rate of outgoing said used dehydration alcohol that is concomitantly expelled as said used dehydration alcohol from said SOP separator. The precise temperature of said dehydration alcohol and the precise flow rate of incoming said dehydration alcohol are variables which may be modified in order to optimize the efficiency and productivity of said basic SOP process in relation to the species of raw plant tissue and the conditions and equipment available. Following completion of said spraying, said washed secondary SOP is spun in said vertical basket providing said constant centripetal force for five additional minutes while continuing to expel said used dehydration alcohol from said SOP separator within conduit(s), using valves and pumps as necessary, to a suitable storage tank in support of its subsequent distillation, said distillation being to separate and recover said aliphatic alcohol. Said vertical basket is then decelerated to zero angular velocity, and said dehydrated secondary SOP and said SOP filter are removed from said SOP separator for storage or further processing as desired.
Following transfer of said entire volume of said dispersed secondary suspension from said SOP-forming tank to said SOP separator during production of said cakes of secondary SOP, the walls of said SOP-forming tank are washed to produce clean SOP-forming tank. Said clean SOP-forming tank is produced by washing the walls of said SOP-forming tank with said secondary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed secondary suspension from said SOP-forming tank to said SOP
separator. While washing said walls of said SOP-forming tank, said secondary washing solution is expelled from said SOP-forming tank via said outlet ports of said SOP-forming tank into said non-valved conduit(s) and transferred through said non-valved conduit(s) to and through said inlet(s) into said SOP separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary. After said washing of said walls of said SOP-forming tank with said secondary washing solution and expelling of said secondary washing solution from said SOP-forming tank, cleaning of said non-valved conduit(s) between said SOP-forming tank and said SOP separator is done. Said cleaning is accomplished by introducing into said SOP-forming tank and said outlet ports of said SOP-forming tank said secondary washing solution at said ambient or lower temperature and of volume no less than three times the volume contained by those said non-valved conduit(s) used to transfer said dispersed secondary suspension from said SOP-forming tank to said SOP separator at a flow rate regulated to match the rate of removal of liquids from said outlet(s), using pumps as necessary.
After completion of said cleaning, said non-valved conduit(s) between said SOP-forming tank and said SOP separator is disconnected from said inlet(s) leading into said SOP
separator, and flushing of said SOP-forming tank and said non-valved conduit(s) is done.
Said flushing is accomplished by introducing into said SOP-forming tank liquid water having a temperature below the boiling point for outflow of said liquid water through said outlet ports of said SOP-forming tank hence through said non-valved conduit(s). Said flushing is continued until clear water flows freely from the disconnected end(s) of said non-valved conduit(s).
Cakes of SOP, whether of primary or secondary designation, bleached or unbleached, hydrated or partially dehydrated, as produced in said basic SOP process are miscible in water upon stirring. A
clear solution of water miscible oligosaccharides and polysaccharides, here designated as MOP, is produced by weighing a mass of said SOP and adding to said mass a volume in litres of water equaling at least twice the mass in kilograms of said SOP, followed by stirring the mixture at said ambient pressure and a temperature between 0 oC and 100 oC until a clear solution is obtained. The precise temperature of said stirring to produce said MOP is a variable which may be modified in order to optimize the efficiency and productivity of the process in relation to the species of raw plant tissue and the conditions and equipment available. Said MOP is a convenient way to transport and further refine SOP.
Said distillation is specified as part of the overall said basic SOP process, and said distillation is done in a distillation apparatus in order to recover and, if so desired, to recycle said aliphatic alcohol. Said distillation is not essential for production of SOP
using said basic SOP process, but said distillation serves to prevent the environmental contamination which might otherwise occur, and said distillation also presents the opportunity for the aqueous residue remaining after said distillation also to be used again. Recovery by volume of said aliphatic alcohol during said distillation is in the range of 85 - 95% of the volumes of said aliphatic alcohol introduced into said SOP forming tank to produce said primary suspension and said secondary suspension. If said distillation employs boiling at ambient pressure at or near the boiling temperature of said aliphatic alcohol, said aliphatic alcohol is recovered in marginally higher yield than if said distillation employs vacuum distillation at a temperature below the ambient boiling temperature.
Said aqueous residue remaining after said distillation can be transferred via conduit(s), using pumps and valves as necessary, from said distillation apparatus to fill an alkali storage tank to a known volume. Said alkali storage tank must be capable of stirring and/or mixing its contents at said ambient temperature and pressure. Said aqueous residue transferred from said distillation apparatus into said alkali storage tank is titrated for its alkaline hydroxide content followed by addition to said aqueous residue sufficient amount of said alkaline hydroxide to produce alkaline soaking solution that fulfils the specified requirement of said known concentration of said primary soaking solution or said secondary soaking solution. From said alkali storage tank, said alkaline soaking solution is transferred to said extraction vessel to achieve a said primary soak or a said secondary soak of another batch of said pieces of raw plant tissue of dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length. In this way, said aqueous residue can be recycled through said basic SOP process.
Following repeated recycling of said aqueous residue in support of the production of successive batches of SOP using said basic SOP process, an insoluble precipitate forms in said aqueous residue within said distillation apparatus during or after said distillation. Said insoluble precipitate is formed from substances which were extracted from said pieces of raw plant tissue and/or from said insoluble residue of said pieces of raw plant tissue during said primary soak and/or said secondary soak, respectively. Said insoluble precipitate comprises chemical substances potentially of high economic value and, following removal from said distillation apparatus of the clear liquid component of said aqueous residue, said insoluble precipitate remaining in said distillation apparatus may be recovered either by physical means or by dissolving said insoluble precipitate in an appropriate solvent and removing that solution, simultaneously cleaning said distillation unit. Said clear liquid component of said aqueous residue is transferred via conduit(s), using pumps and valves as necessary, from said distillation apparatus to fill to a known volume said alkali storage tank capable of stirring and/or mixing its contents at ambient temperature and pressure. Said clear liquid component of said aqueous residue transferred from said distillation apparatus into said alkali storage tank is titrated for its alkaline hydroxide content followed by addition to said aqueous residue sufficient amount of said alkaline hydroxide to produce alkaline soaking solution that fulfils the specified requirement of said known concentration of said primary soaking solution or said secondary soaking solution. From said alkali storage tank, said alkaline soaking solution is transferred to said extraction vessel to achieve a said primary soak or a said secondary soak of another batch of said pieces of raw plant tissue of dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length.
If disposal into the environment rather than recycling of said aqueous residue is opted for, it deserves emphasis that said aqueous residue is enriched in alkaline hydroxide content and therefore is potentially harmful to life if not first neutralized and desalted by some means, for example, by addition of acid to lower the pH and enable removal of the high salt concentration.
A number of variables potentially affecting SOP yield and/or cost are listed below in relation to production of said number one bleached dehydrated SOP, only, but this listing also serves to reveal the broad methodological versatility available to said basic SOP process in relation to production of SOP in general. A non-comprehensive list of said variables includes the following:
1) said plant species which is processed;
2) anatomical and chemical composition including water content of said raw pieces of plant tissue processed;
3) kind and size of said extraction vessel used;
4) alkaline hydroxide metal(s), viz., sodium potassium, lithium, selected for use in said primary soaking solution;
5) said known concentration of said alkaline hydroxide used in said primary soaking solution;
6) duration of said primary soaking time in said extraction vessel;
7) temperature of said primary soaking solution in said extraction vessel;
8) method used to displace and transfer said primary soaking solution from said extraction vessel to said SOP-forming tank;
9) respecting said conduit(s) between said extraction vessel and said SOP-forming tank, said conduit(s) between said SOP-forming tank and said SOP separator, and said conduit(s) between said SOP separator and tanks receiving solutions expelled from said SOP separator, all must be compatible with said alkaline hydroxide and said aliphatic alcohol and, therefore, it is recommended that all be of inert plastic;
however, shape, wall thickness, and dimensions of said conduit(s) are not specified here;
10) non-specified features of said SOP forming tank;
11) kind of said aliphatic alcohol added to said SOP forming tank to produce said primary suspension;
12) duration of said mixing time in said SOP forming tank to produce said primary mixture;
13) method and intensity of mixing to achieve said primary mixture in said SOP
forming tank;
14) duration of said setting time to produce said primary suspension;
15) nature of said SOP separator and said SOP filter;
16) physical environment setpoints used during separation of SOP batch number one from the 1:1 (v/v) mixture of alkaline soaking solution and aliphatic alcohol;
17) duration of washing, bleaching, rinsing and dehydrating the SOP cake.
Example Data arising from application of said basic SOP process to pieces of wood from Betula populifolia are presented herewith in Figure 1 and Tables 1-11, and data on SOP yields from tissues of a number of additional plant species using said basic SOP process are also presented in Tables 11 and 12. However, said data are not to specify that said basic SOP
process as stated for B. populifolia and said additional plant species must be rigidly adhered to for either those or other plant species. Using said basic SOP process, some quantity of SOP evidently can be obtained from any tissue of any plant species, and the methodological latitude within said basic SOP process invites modifications in order to increase SOP yield and reduce costs.
The chemistry of SOP from Betula populifolia wood was investigated in some depth, by dialysis followed by sulfuric acid hydrolysis of the SOP followed by barium carbonate neutralization, drying, trimethylsilylation and analysis by combined gas chromatography -mass spectroscopy (GC/ MS). Dialysis through cellulose acetate of different molecular-weight cutoffs established that B. populifolia SOP comprises a small fraction of short-chain oligosaccharides as well as larger polysaccharides, the major fraction being above 10,000 Daltons. GC/MS analysis of hydrolyzed, trimethylsilylated SOP revealed that B.
populifolia SOP contains equal amounts of D-xylose and 4-mefftylglucuronic acid as its dominant building blocks. Those two compounds are well known constituents of Magnoliophyta hemicelluloses, and thus said basic SOP process is a simple and rapid method to mass produce those two compounds. However, considerable research remains to be done in order to understand the chemistry of SOP as it may vary among plant species.
Data on SOP production from wood of Betula populifolia using the basic SOP
process.
Figure 1. Percentage yield of SOP from dry, raw wood of Betula populifolia as a function of temperature and NaOH molarity.
Linear twater (control)) 4.
- - Linear OM Na011) SOP
yield ¨ Poly. t2.5M NaOH) (A) 15 - - - - Poly. (5M Na011) 10.e = === = µ*.
=
= = 111 5= , = ' ====
-r0 = ................................................. 4 Extraction temperature ( C) Table 1. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles for different time periods with 1 M NaOH at 25 oC; standard deviations (s.d.) are for 3 replicate investigations.
Time (hours) % SOPs.d.
0.1 <0.1 0.0 1 7.6 0.2 2 7.5 0.4 3 8.3 0.4 4 7.6 0.3 Table 2. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles for 1 hour at 50 0C at different NaOH
molarities; standard deviations (s.d.) are for 3 replicate investigations.
NaOH
molarity % SOPs.d.
water only 0.3 0.0 1.0 4.6 0.1 2.5 14.7 0.3 5.0 11.2 0.6 10.0 13.2 0.3 Table 3. Dehydrated SOP yields (% of dry, raw wood weight) after extracting different sizes of dry, raw Betula populifolia wood particles once or twice for different time periods with 2.5 M NaOH at 50 0C; standard deviations (s.d.) are for 3 replicate investigations.
Maximum particle surface area dimension (mm) (mm2/ gram) % SOPs.d.
3.5 4160 16.0 0.5 130 1600 5.8 0.1 136 1280 5.8 0.2 176 1120 4.6 0.6 Table 4. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles once or twice for different time periods with 2.5 M NaOH at 50 oC; standard deviations (s.d.) are for 3 replicate investigations.
No. of times extracted Time (hours) % SOP s.d.
once 1 12.8 0.4 twice 1, 1 17.3 0.3 twice 0.1, 1 16.3 0.5 once 0.165 9.9 0.4 once 1.165 13.0 0.6 Table 5. Dehydrated SOP yields (% of dry, raw wood weight) as influenced by the aliphatic alcohol used, after extracting dry, raw Betula populifolia wood partides with 2.5 M NaOH for one hour at 50 0C; and adding an equal volume of an aliphatic alcohol to generate a SOP
suspension; standard deviations (s.d.) are for 3 replicate investigations.
Aliphatic alcohol % SOPs.d.
ethanol 15.3 0.3 methanol 11.5 0.4 2-propanol 6.7 0.3 n-butanol 5.2 0.1 Table 6. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles with 1.0 M NaOH or 2.5 M NaOH at 50 0C and adding the indicated volume of ethanol to generate a SOP suspension; standard deviations (s.d.) are for 3 replicate investigations.
1.0 M NaOH 2.5 M NaOH
% (v/v) ethanol % SOPs.d. % SOP s.d.
50% 6.0 0.2 23.0 1.4 67% 7.4 0.3 21.5 1.1 Table 7. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood partides with three kinds of alkali at 1.0 M or 2.5 M
concentrations for 1 hour at 50 0C; standard deviations (s.d.) are based on 3 replicate investigations.
Alkali % SOP (1.0 M) s.d. % SOP (2.5 M) s.d.
NaOH 4.3 0.3 15.9 0.7 KOH 4.9 0.0 13.8 0.5 LiOH 9.1 0.6 12.1 0.2 Table 8. Yields (% of weight of dry, raw Betula populifolia wood partides) of unbleached and bleached (3% H202 for 10 minutes at ambient temperature) dehydrated SOP
retained by a cellulosic filter following centrifugation at 500 X g; standard deviations (s.d.) are for 3 replicate investigations.
Suspension % SOPs.d.
SOP in 50% 14.9 0.8 ethanol, 2.5 M NaOH
SOP in 3% H202, 50% 8.8 1.0 ethanol, 2.5 M NaOH
Table 9. Weight change of dehydrated SOP (% of the weight of dehydrated Betula populifolia raw SOP based on the yield provided using 50% ethanol) in relation to incremental increases in ethanol concentration during centrifugation, always in the presence of 2.5 M NaOH;
standard deviations (s.d.) are for 3 replicate investigations.
% ethanol weight % s.d.
60 97.6 0.1 70 86.1 0.3 80 90.5 0.2 90 96.2 0.2 95 95.9 0.4 Table 10. SOP recovery as a function of ethanol concentration in water in relation to the process of stepwise ethanolic dehydration of SOP
Ethanol (% v/v) SOP recovery (%) Table 11. Bleached (3% H202 with 47% ethanol and 50% water for 10 minutes at ambient temperature) and unbleached dehydrated SOP yields (% of weight of dry, raw wood particles) from woods of several tree species; standard deviations (s.d.) are for 3 replicate investigations.
Tree species unbleached SOP (%) s.d. bleached SOP (%) s.d.
Betula populifolia 12.5 0.7 9.0 0.3 Betula alleghaniensis 10.4 0.0 9.4 0.3 Acer rubrum 7.2 0.6 6.4 0.1 Populus tremuloides 9.5 0.2 7.6 0.1 Table 12. Average dehydrated SOP yields (% of dry, raw weight based on three replicate preparations) found for various plant species are shown beside each in parentheses. Tissues were extracted with 2.5 M NaOH for 1 hour at 50 0C followed by SOP
precipitation using 50% (v/v) ethanol.
Woods from tree species:
Acacia koa (15.7), Acer saccharum (6.0), Acer saccharinum (10.5), Araucaria heterophylla (1.2), Betula lutea (6.2), Betula populifolia (22.7), Canja pallida (5.6), Corylus avellana (3.8), Dalbergia latifolia (3.1), Diospyros melanoxylon (3.8), Eucalyptus camaldulensis (4.8), Eucalyptus deanii (5.3), Eucalyptus globulus (14.6), Fraxinus americana (5.0), Guaiacum officinale (3.1), Juglans cinerea (19.2), Juglans nigra, Khaya ivorensis (10.2), Liquidambar styraciflua (8.0), Ochroma pyramidales (14.1), Paulownia tomentosa (12.0), Platanus occidentalis (12.6), Podocarpus guatmalensis (1.7), Prunus serotina (15.8), Pterocarpus indicus (3.2), Quercus alba (9.4), Quercus robur (16.1), Quercus rubra (8.0), Salix fragilis (10.6), Swietenia macrophylla (15.0), Tectona grandis (2.6), Terminalia superb (4.6), Terminalia tomentosa (3.9), Turraean thus africana (1.8), Ulmus americana(4.9).
Stems, leaves and reproductive structures: Achillea millefolium (20.6), Bambusa oldhamii (40.2), Gossypium hirsutum (0.2), Hypericum perforatum (28.8), Melilotus alba (16.8), Phalaris arundinacea (39.3), Phleum pretense (31.6), Solidago juncea (21.7).
=
= = 111 5= , = ' ====
-r0 = ................................................. 4 Extraction temperature ( C) Table 1. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles for different time periods with 1 M NaOH at 25 oC; standard deviations (s.d.) are for 3 replicate investigations.
Time (hours) % SOPs.d.
0.1 <0.1 0.0 1 7.6 0.2 2 7.5 0.4 3 8.3 0.4 4 7.6 0.3 Table 2. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles for 1 hour at 50 0C at different NaOH
molarities; standard deviations (s.d.) are for 3 replicate investigations.
NaOH
molarity % SOPs.d.
water only 0.3 0.0 1.0 4.6 0.1 2.5 14.7 0.3 5.0 11.2 0.6 10.0 13.2 0.3 Table 3. Dehydrated SOP yields (% of dry, raw wood weight) after extracting different sizes of dry, raw Betula populifolia wood particles once or twice for different time periods with 2.5 M NaOH at 50 0C; standard deviations (s.d.) are for 3 replicate investigations.
Maximum particle surface area dimension (mm) (mm2/ gram) % SOPs.d.
3.5 4160 16.0 0.5 130 1600 5.8 0.1 136 1280 5.8 0.2 176 1120 4.6 0.6 Table 4. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles once or twice for different time periods with 2.5 M NaOH at 50 oC; standard deviations (s.d.) are for 3 replicate investigations.
No. of times extracted Time (hours) % SOP s.d.
once 1 12.8 0.4 twice 1, 1 17.3 0.3 twice 0.1, 1 16.3 0.5 once 0.165 9.9 0.4 once 1.165 13.0 0.6 Table 5. Dehydrated SOP yields (% of dry, raw wood weight) as influenced by the aliphatic alcohol used, after extracting dry, raw Betula populifolia wood partides with 2.5 M NaOH for one hour at 50 0C; and adding an equal volume of an aliphatic alcohol to generate a SOP
suspension; standard deviations (s.d.) are for 3 replicate investigations.
Aliphatic alcohol % SOPs.d.
ethanol 15.3 0.3 methanol 11.5 0.4 2-propanol 6.7 0.3 n-butanol 5.2 0.1 Table 6. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood particles with 1.0 M NaOH or 2.5 M NaOH at 50 0C and adding the indicated volume of ethanol to generate a SOP suspension; standard deviations (s.d.) are for 3 replicate investigations.
1.0 M NaOH 2.5 M NaOH
% (v/v) ethanol % SOPs.d. % SOP s.d.
50% 6.0 0.2 23.0 1.4 67% 7.4 0.3 21.5 1.1 Table 7. Dehydrated SOP yields (% of dry, raw wood weight) after extracting dry, raw Betula populifolia wood partides with three kinds of alkali at 1.0 M or 2.5 M
concentrations for 1 hour at 50 0C; standard deviations (s.d.) are based on 3 replicate investigations.
Alkali % SOP (1.0 M) s.d. % SOP (2.5 M) s.d.
NaOH 4.3 0.3 15.9 0.7 KOH 4.9 0.0 13.8 0.5 LiOH 9.1 0.6 12.1 0.2 Table 8. Yields (% of weight of dry, raw Betula populifolia wood partides) of unbleached and bleached (3% H202 for 10 minutes at ambient temperature) dehydrated SOP
retained by a cellulosic filter following centrifugation at 500 X g; standard deviations (s.d.) are for 3 replicate investigations.
Suspension % SOPs.d.
SOP in 50% 14.9 0.8 ethanol, 2.5 M NaOH
SOP in 3% H202, 50% 8.8 1.0 ethanol, 2.5 M NaOH
Table 9. Weight change of dehydrated SOP (% of the weight of dehydrated Betula populifolia raw SOP based on the yield provided using 50% ethanol) in relation to incremental increases in ethanol concentration during centrifugation, always in the presence of 2.5 M NaOH;
standard deviations (s.d.) are for 3 replicate investigations.
% ethanol weight % s.d.
60 97.6 0.1 70 86.1 0.3 80 90.5 0.2 90 96.2 0.2 95 95.9 0.4 Table 10. SOP recovery as a function of ethanol concentration in water in relation to the process of stepwise ethanolic dehydration of SOP
Ethanol (% v/v) SOP recovery (%) Table 11. Bleached (3% H202 with 47% ethanol and 50% water for 10 minutes at ambient temperature) and unbleached dehydrated SOP yields (% of weight of dry, raw wood particles) from woods of several tree species; standard deviations (s.d.) are for 3 replicate investigations.
Tree species unbleached SOP (%) s.d. bleached SOP (%) s.d.
Betula populifolia 12.5 0.7 9.0 0.3 Betula alleghaniensis 10.4 0.0 9.4 0.3 Acer rubrum 7.2 0.6 6.4 0.1 Populus tremuloides 9.5 0.2 7.6 0.1 Table 12. Average dehydrated SOP yields (% of dry, raw weight based on three replicate preparations) found for various plant species are shown beside each in parentheses. Tissues were extracted with 2.5 M NaOH for 1 hour at 50 0C followed by SOP
precipitation using 50% (v/v) ethanol.
Woods from tree species:
Acacia koa (15.7), Acer saccharum (6.0), Acer saccharinum (10.5), Araucaria heterophylla (1.2), Betula lutea (6.2), Betula populifolia (22.7), Canja pallida (5.6), Corylus avellana (3.8), Dalbergia latifolia (3.1), Diospyros melanoxylon (3.8), Eucalyptus camaldulensis (4.8), Eucalyptus deanii (5.3), Eucalyptus globulus (14.6), Fraxinus americana (5.0), Guaiacum officinale (3.1), Juglans cinerea (19.2), Juglans nigra, Khaya ivorensis (10.2), Liquidambar styraciflua (8.0), Ochroma pyramidales (14.1), Paulownia tomentosa (12.0), Platanus occidentalis (12.6), Podocarpus guatmalensis (1.7), Prunus serotina (15.8), Pterocarpus indicus (3.2), Quercus alba (9.4), Quercus robur (16.1), Quercus rubra (8.0), Salix fragilis (10.6), Swietenia macrophylla (15.0), Tectona grandis (2.6), Terminalia superb (4.6), Terminalia tomentosa (3.9), Turraean thus africana (1.8), Ulmus americana(4.9).
Stems, leaves and reproductive structures: Achillea millefolium (20.6), Bambusa oldhamii (40.2), Gossypium hirsutum (0.2), Hypericum perforatum (28.8), Melilotus alba (16.8), Phalaris arundinacea (39.3), Phleum pretense (31.6), Solidago juncea (21.7).
Claims (60)
1. A process for producing from pieces of raw plant tissue and alkaline soaking solution during soda, kraft, alkaline sulfite or any other industry of chemical or semi-chemical alkaline-pulping, or any other industry operating independently of the pulping industry, a fluid suspension of coagulated substances containing oligosaccharides and polysaccharides, involving in addition to said pieces of raw plant tissue and said alkaline soaking solution an extraction vessel, a solid oligosaccharides and polysaccharides - forming tank (SOP-forming tank), conduit(s) between said extraction vessel and said SOP-forming tank, liquid aliphatic alcohol pre-chilled to a temperature at least 10 °C below its flash point, and the recovered volume of said alkaline soaking solution, comprising the steps of:
a) loading into said extraction vessel a full or lesser load of said pieces of raw plant tissue under ambient temperature and pressure conditions;
b) introducing into said extraction vessel loaded with said pieces of raw plant tissue under ambient temperature and pressure conditions said alkaline soaking solution having a desired concentration, selected from within the range 0.5 - 10 M, of an alkaline hydroxide in aqueous solution, said alkaline soaking solution is introduced in sufficient or greater volume to achieve a soak of all said pieces of raw plant tissue in said extraction vessel;
c) maintaining said pieces of raw plant tissue of step (a) soaking in said alkaline soaking solution of step (b) for a defined time selected from within the range 0.1 - 4.0 hours at a temperature selected from within the range 4 - 100 °C;
d) expelling a recovered volume of said alkaline soaking solution from said extraction vessel into conduit(s), using pumps and valves as necessary;
e) transferring said recovered volume of said alkaline soaking solution from said extraction vessel via said conduit(s), using pumps and valves as necessary, to said SOP-forming tank, concomitantly maintaining within said extraction vessel the residue of said pieces of raw plant tissue that were loaded during step (a);
f) measuring said recovered volume within said SOP-forming tank;
g) adding to said SOP-forming tank a volume of said liquid aliphatic alcohol equaling that of said recovered volume, said aliphatic alcohol is added to said recovered volume within said SOP-forming tank until the total volume of liquid contained in said SOP-forming tank is twice, within volumetric precision of 2%, that of said recovered volume, said liquid aliphatic alcohol is of no less than 95% purity and contains by volume 5% or less water;
h) mixing said liquid aliphatic alcohol with said recovered volume of said alkaline soaking solution within said SOP-forming tank for a mixing time, selected from the range 1 - 30 minutes, sufficient to achieve uniform mixing thus producing a 1:1 (v/v) homogeneous mixture of said recovered volume of said alkaline soaking solution and the equivalent volume of said liquid aliphatic alcohol;
i) setting the 1:1 (v/v) homogeneous mixture of step (h) under static conditions for a setting time selected from the range 0.1 - 24 hours, during the course of said setting time, there forms said fluid suspension of coagulated substances containing oligosaccharides and polysaccharides.
a) loading into said extraction vessel a full or lesser load of said pieces of raw plant tissue under ambient temperature and pressure conditions;
b) introducing into said extraction vessel loaded with said pieces of raw plant tissue under ambient temperature and pressure conditions said alkaline soaking solution having a desired concentration, selected from within the range 0.5 - 10 M, of an alkaline hydroxide in aqueous solution, said alkaline soaking solution is introduced in sufficient or greater volume to achieve a soak of all said pieces of raw plant tissue in said extraction vessel;
c) maintaining said pieces of raw plant tissue of step (a) soaking in said alkaline soaking solution of step (b) for a defined time selected from within the range 0.1 - 4.0 hours at a temperature selected from within the range 4 - 100 °C;
d) expelling a recovered volume of said alkaline soaking solution from said extraction vessel into conduit(s), using pumps and valves as necessary;
e) transferring said recovered volume of said alkaline soaking solution from said extraction vessel via said conduit(s), using pumps and valves as necessary, to said SOP-forming tank, concomitantly maintaining within said extraction vessel the residue of said pieces of raw plant tissue that were loaded during step (a);
f) measuring said recovered volume within said SOP-forming tank;
g) adding to said SOP-forming tank a volume of said liquid aliphatic alcohol equaling that of said recovered volume, said aliphatic alcohol is added to said recovered volume within said SOP-forming tank until the total volume of liquid contained in said SOP-forming tank is twice, within volumetric precision of 2%, that of said recovered volume, said liquid aliphatic alcohol is of no less than 95% purity and contains by volume 5% or less water;
h) mixing said liquid aliphatic alcohol with said recovered volume of said alkaline soaking solution within said SOP-forming tank for a mixing time, selected from the range 1 - 30 minutes, sufficient to achieve uniform mixing thus producing a 1:1 (v/v) homogeneous mixture of said recovered volume of said alkaline soaking solution and the equivalent volume of said liquid aliphatic alcohol;
i) setting the 1:1 (v/v) homogeneous mixture of step (h) under static conditions for a setting time selected from the range 0.1 - 24 hours, during the course of said setting time, there forms said fluid suspension of coagulated substances containing oligosaccharides and polysaccharides.
2. The process of Claim 1 wherein said pieces of raw plant tissue have dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length and are wood obtained from any of the following plant species: Acacia koa, Acer saccharum, Acer saccharinum, Araucaria heterophylla, Betula lutea, Betula populifolia, Carya pallida, Corylus avellana, Dalbergia latifolia, Diospyros melanoxylon, Eucalyptus camaldulensis, Eucalyptus deanii, Eucalyptus globulus, Fraxinus americana, Guaiacum officinale, Juglans cinerea, Juglans nigra, Khaya ivorensis, Liquidambar styraciflua, Ochroma pyramidales, Paulownia tomentosa, Platanus occidentalis, Podocarpus guatmalensis, Prunus serotina, Pterocarpus indicus, Quercus alba, Quercus robur, Quercus rubra, Salix fragilis, Swietenia macrophylla, Tectona grandis, Terminalia superba, Terminalia tomentosa, Turraer~hus africana, Ulmus americana.
3. The process of Claim 1 wherein said pieces of raw plant tissue have dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length and are wood obtained from any plant species.
4. The process of Claim 1 wherein said pieces of raw plant tissue have dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length and comprise stem, leaf or reproductive tissues obtained from any of the following plant species:
Achillea millefolium, Bambusa oldhamii, Gossypium hirsi~, Hypericum perforatum, Melilotus alba, Phalaris arundinacea, Phleum pretense, Solidago juncea.
Achillea millefolium, Bambusa oldhamii, Gossypium hirsi~, Hypericum perforatum, Melilotus alba, Phalaris arundinacea, Phleum pretense, Solidago juncea.
5. The process of Claim 1 wherein said pieces of raw plant tissue have dimensions up to or less than 10 mm in thickness, 10 mm in width and 50 mm in length and comprise stem, leaf or fruit tissues obtained from any plant species.
6. The process of Claim 1 wherein said extraction vessel is a pulp-mill batch digester.
7. The process of Claim 1 wherein said extraction vessel is any container that is loaded with said pieces of raw plant tissue and said alkaline soaking solution, providing and tolerating the soaking conditions, discharging said alkaline soaking solution independently of the insoluble residue of said pieces of raw plant tissue, and being unloaded of said insoluble residue.
8. The process of Claim 1 wherein said alkaline hydroxide is sodium hydroxide.
9. The process of Claim 1 wherein said alkaline hydroxide is potassium hydroxide.
10. The process of Claim 1 wherein said alkaline hydroxide is lithium hydroxide.
11. The process of Claim 1 wherein said SOP-forming tank is a container compatible with said alkaline soaking solution and said aliphatic alcohol and equipped with several devices, viz., a device for accurately measuring and indicating the volume of contained liquid within said SOP-forming tank, a refrigeration unit for cooling the internal environment, thermometers for accurately measuring the temperature of said contained liquid and air above said contained liquid, mechanism(s) to stir and/or mix said contained liquid, intake and outlet ports and pumps for receiving and discharging liquids and suspensions, respectively, and additional devices needed to regulate rates of stirring and/or mixing, receiving and discharging of both incoming liquids and outward flowing suspensions.
12. The process of Claim 1 wherein the volume capacity of said SOP-forming tank is greater than twice the volume of said recovered volume of said alkaline soaking solution.
13. The process of Claim 1 wherein said aliphatic alcohol is ethanol, otherwise known as ethyl alcohol, grain alcohol, hydroxyethane or ethyl hydrate.
14. The process of Claim 1 wherein said aliphatic alcohol is methanol, otherwise known as methyl alcohol, hydroxymethane, methyl hydrate, wood alcohol or carbinol.
15. The process of Claim 1 wherein said aliphatic alcohol is 2-propanol, otherwise known as iso-propanol, isopropyl alcohol or propan-2-ol.
16. The process of Claim 1 wherein said aliphatic alcohol is n-butanol, otherwise known as normal butanol, butyl alcohol, butyric alcohol, propylcarbinol, 1-butanol, or butan-1-ol.
17. The process of Claim 1 wherein said aliphatic alcohol added to said alkaline extracting solution in said SOP-forming tank is any volumetric combination of ethanol, methanol, 2-propanol and n-butanol.
18. The process of Claim 1 wherein steps (b), (c), (d), (e), (f), (g), (h) and (i) are repeated.
19. A process for separating solid oligosaccharides and polysaccharides (SOP) from a clear liquid of a fluid suspension, retaining and accumulating a cake of SOP within a solid oligosaccharides and polysaccharides separator (SOP separator) having inlet(s) to receive said fluid suspension or other liquids, outlet(s) for removing liquid from said SOP separator and a filter passing said clear liquid and retaining said cake of SOP, and transferring said clear liquid via valved conduit(s) to a storage container, comprising the steps of:
a) introducing said fluid suspension as a uniformly dispersed suspension through said inlet(s) into said SOP separator;
b) applying a force selected from within the range 1 X ~ to 500 X ~, ~ being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2, to said fluid suspension in order to force said clear liquid through said filter and enable said clear liquid to be expelled through said outlet(s); and c) removing said clear liquid expelled from said outlet(s) and transferring said clear liquid via said valved conduit(s) to said storage container, using valves and pumps for the transfer.
a) introducing said fluid suspension as a uniformly dispersed suspension through said inlet(s) into said SOP separator;
b) applying a force selected from within the range 1 X ~ to 500 X ~, ~ being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2, to said fluid suspension in order to force said clear liquid through said filter and enable said clear liquid to be expelled through said outlet(s); and c) removing said clear liquid expelled from said outlet(s) and transferring said clear liquid via said valved conduit(s) to said storage container, using valves and pumps for the transfer.
20. The process of Claim 19 wherein said SOP separator is a centrifuge.
21. The process of Claim 19 wherein said SOP separator is a modified clothes washing machine.
22. The process of Claim 19 wherein said SOP separator is a positive pressure filtration system.
23. The process of Claim 19 wherein said SOP separator is a vacuum filtration system.
24. The process of Claim 19 wherein said SOP separator is a gravity-flow filtration system.
25. The process of Claim 19 wherein said SOP separator has at least one said inlet(s) that may be opened or closed and at least one said outlet(s) that may be opened or closed to permit said fluid suspension or other liquid to enter and exit, respectively.
26. The process of Claim 19 wherein said filter contains cellulose and does not retain particles having smallest dimension less than 1~ µm.
27. The process of Claim 19 wherein said valved conduit(s) is chemically and physically compatible with the process and uses pumps and regulators.
28. A process for washing, bleaching, rinsing, and partial dehydrating a cake of solid oligosaccharides and polysaccharides (SOP) within a solid oligosaccharides and polysaccharides separator (SOP separator) by introducing through at least one inlet of said SOP separator washing solution, bleaching solution, rinsing solution and dehydration alcohol, concomitantly expelling through a filter and at least one outlet of said SOP separator used washing solution, used bleaching solution, used rinsing solution and used dehydration alcohol and transferring said used washing solution, said used bleaching solution, said used rinsing solution and said used dehydration alcohol via at least one valved conduit, using pumps and valves, to appropriate storage container, comprising the steps of:
a) washing said cake of SOP with washing solution comprising 1:1 (v/v) mixture of water and an aliphatic alcohol for a washing time selected from the range 0.2 -1.0 hour, wherein to initiate said washing, said at least one outlet is closed, and said washing solution is introduced through said at least one inlet into said SOP separator in sufficient volume to fill said SOP separator to its operational capacity, then said at least one outlet is opened and said expelling of said used washing solution through said at least one outlet is begun using force from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2; and wherein after said used washing solution has been expelled through said at least one outlet to the extent that said cake no longer appears wet, additional said washing solution is introduced through said at least one inlet to re-wet said cake, and the resulting said used washing solution is expelled using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2, through said at least one outlet to said storage container at a flow rate equal to or greater than the rate that said washing solution is introduced through said at least one inlet;
b) bleaching said cake of SOP with said bleaching solution comprising by volume a percentage of hydrogen peroxide selected from the range 3 - 10% (v/v) , 50%
said aliphatic alcohol and the balance water for a bleaching time selected from the range 0.2 - 1.0 hour, wherein to initiate said bleaching, said at least one outlet is closed, and said bleaching solution is introduced through said at least one inlet into said SOP
separator in sufficient volume to fill said SOP separator to its operational capacity, then said at least one inlet is closed and said cake of SOP is incubated in said bleaching solution for an elected bleaching time, and wherein following elapse of the elected bleaching time, said at least one outlet is opened and said expelling of said used bleaching solution through said at least one outlet occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2 until said cake no longer appears wet;
c) rinsing said cake of SOP with said rinsing solution comprising 1:1 (v/v) mixture of water and said aliphatic alcohol for a rinsing time selected from the range five to thirty minutes, wherein to initiate said rinsing, said at least one outlet is opened, and said rinsing solution is continuously introduced through said at least one inlet into said SOP separator as said expelling of said used rinsing solution through said at least one outlet concomitantly occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m S-2 such that the flow rate through the at least one inlet is equal to or less than the rate that said rinsing solution is expelled through said at least one outlet;
d) partial dehydrating for five minutes or less said cake of SOP using said dehydration alcohol being said aliphatic alcohol containing 5% or less water content and pre-chilled to a temperature at least 10 °C below the flash point of said dehydration alcohol, wherein to initiate said partial dehydrating, said at least one outlet is opened, and said dehydration alcohol is continuously introduced through said at least one inlet into said SOP separator as said expelling of said used dehydration alcohol through said at least one outlet concomitantly occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m S-2 such that the flow rate through the at least one inlet is equal to or less than the rate that said dehydration alcohol is expelled through said at least one outlet.
a) washing said cake of SOP with washing solution comprising 1:1 (v/v) mixture of water and an aliphatic alcohol for a washing time selected from the range 0.2 -1.0 hour, wherein to initiate said washing, said at least one outlet is closed, and said washing solution is introduced through said at least one inlet into said SOP separator in sufficient volume to fill said SOP separator to its operational capacity, then said at least one outlet is opened and said expelling of said used washing solution through said at least one outlet is begun using force from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2; and wherein after said used washing solution has been expelled through said at least one outlet to the extent that said cake no longer appears wet, additional said washing solution is introduced through said at least one inlet to re-wet said cake, and the resulting said used washing solution is expelled using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2, through said at least one outlet to said storage container at a flow rate equal to or greater than the rate that said washing solution is introduced through said at least one inlet;
b) bleaching said cake of SOP with said bleaching solution comprising by volume a percentage of hydrogen peroxide selected from the range 3 - 10% (v/v) , 50%
said aliphatic alcohol and the balance water for a bleaching time selected from the range 0.2 - 1.0 hour, wherein to initiate said bleaching, said at least one outlet is closed, and said bleaching solution is introduced through said at least one inlet into said SOP
separator in sufficient volume to fill said SOP separator to its operational capacity, then said at least one inlet is closed and said cake of SOP is incubated in said bleaching solution for an elected bleaching time, and wherein following elapse of the elected bleaching time, said at least one outlet is opened and said expelling of said used bleaching solution through said at least one outlet occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2 until said cake no longer appears wet;
c) rinsing said cake of SOP with said rinsing solution comprising 1:1 (v/v) mixture of water and said aliphatic alcohol for a rinsing time selected from the range five to thirty minutes, wherein to initiate said rinsing, said at least one outlet is opened, and said rinsing solution is continuously introduced through said at least one inlet into said SOP separator as said expelling of said used rinsing solution through said at least one outlet concomitantly occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m S-2 such that the flow rate through the at least one inlet is equal to or less than the rate that said rinsing solution is expelled through said at least one outlet;
d) partial dehydrating for five minutes or less said cake of SOP using said dehydration alcohol being said aliphatic alcohol containing 5% or less water content and pre-chilled to a temperature at least 10 °C below the flash point of said dehydration alcohol, wherein to initiate said partial dehydrating, said at least one outlet is opened, and said dehydration alcohol is continuously introduced through said at least one inlet into said SOP separator as said expelling of said used dehydration alcohol through said at least one outlet concomitantly occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m S-2 such that the flow rate through the at least one inlet is equal to or less than the rate that said dehydration alcohol is expelled through said at least one outlet.
29. A process for washing and partial dehydrating a cake of solid oligosaccharides and polysaccharides (SOP) within a solid oligosaccharides and polysaccharides separator (SOP separator) by introducing through at least one inlet of said SOP
separator washing solution and dehydration alcohol, concomitantly expelling through a filter and at least one outlet of said SOP separator used washing solution and used dehydration alcohol and transferring said used washing solution and said used dehydration alcohol via at least one valved conduit, using pumps and valves, to appropriate storage container, comprising the steps of:
a) washing said cake of SOP with washing solution comprising 1:1 (v/v) mixture of water and an aliphatic alcohol for a washing time selected from the range 0.2 -1.0 hour, wherein to initiate said washing, said at least one outlet is closed, and said washing solution is introduced through said at least one inlet into said SOP separator in sufficient volume to fill said SOP separator to its operational capacity, then said at least one outlet is opened and said expelling of said used washing w, don through said at least one outlet is begun using force from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2; and wherein after said used washing solution has been expelled through said at least one outlet to the extent that said cake no longer appears wet, additional said washing solution is introduced through said at least one inlet to re-wet said cake, and the resulting said used washing solution is expelled using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2, through said at least one outlet to said storage container at a flow rate equal to or greater than the rate that said washing solution is introduced through said at least one inlet;
b) partial dehydrating for five minutes or less said cake of SOP using said dehydration alcohol being said aliphatic alcohol containing 5% or less water content and pre-chilled to a temperature at least 10 °C below the flash point of said dehydration alcohol, wherein to initiate said partial dehydrating, said at least one outlet is opened, and said dehydration alcohol is continuously introduced through said at least one inlet into said SOP separator as said expelling of said used dehydration alcohol through said at least one outlet concomitantly occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2 such that the flow rate through the at least one inlet is equal to or less than the rate that said dehydration alcohol is expelled through said at least one outlet.
separator washing solution and dehydration alcohol, concomitantly expelling through a filter and at least one outlet of said SOP separator used washing solution and used dehydration alcohol and transferring said used washing solution and said used dehydration alcohol via at least one valved conduit, using pumps and valves, to appropriate storage container, comprising the steps of:
a) washing said cake of SOP with washing solution comprising 1:1 (v/v) mixture of water and an aliphatic alcohol for a washing time selected from the range 0.2 -1.0 hour, wherein to initiate said washing, said at least one outlet is closed, and said washing solution is introduced through said at least one inlet into said SOP separator in sufficient volume to fill said SOP separator to its operational capacity, then said at least one outlet is opened and said expelling of said used washing w, don through said at least one outlet is begun using force from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2; and wherein after said used washing solution has been expelled through said at least one outlet to the extent that said cake no longer appears wet, additional said washing solution is introduced through said at least one inlet to re-wet said cake, and the resulting said used washing solution is expelled using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2, through said at least one outlet to said storage container at a flow rate equal to or greater than the rate that said washing solution is introduced through said at least one inlet;
b) partial dehydrating for five minutes or less said cake of SOP using said dehydration alcohol being said aliphatic alcohol containing 5% or less water content and pre-chilled to a temperature at least 10 °C below the flash point of said dehydration alcohol, wherein to initiate said partial dehydrating, said at least one outlet is opened, and said dehydration alcohol is continuously introduced through said at least one inlet into said SOP separator as said expelling of said used dehydration alcohol through said at least one outlet concomitantly occurs using force of from within the range 1 X g to 500 X g, g being the nominal acceleration due to gravity on Earth at sea level and equaling approximately 9.8 m s-2 such that the flow rate through the at least one inlet is equal to or less than the rate that said dehydration alcohol is expelled through said at least one outlet.
30. A process for transferring a fluid suspension out of a solid oligosaccharides and polysaccharides-forming tank (SOP-forming tank) into a solid oligosaccharides and polysaccharides separator (SOP separator) via outlet ports and non-valved conduit(s) between said SOP-forming tank and said SOP separator, and for subsequently cleaning said SOP-forming tank and said non-valved conduit(s), comprising the steps of:
a) producing a uniformly dispersed suspension by continuously stirring or mixing said fluid suspension within said SOP-forming tank until such time as said fluid suspension has been expelled from said SCP-forming tank via said outlet ports into said non-valved conduit(s) leading to at least one inlet;
b) expelling to the fullest extent possible all uniformly dispersed suspension of said fluid suspension produced in step (a) within said SOP-forming tank from said SOP-forming tank via said outlet ports into said non-valved conduit(s), using pumps;
c) transferring the uniformly dispersed suspension of said fluid suspension via said non-valved conduit(s) to and through said at least one inlet into said SOP
separator using pumps;
d) washing the walls of said SOP-forming tank thoroughly after completion of step (b) with a washing solution wherein washing is done with a volume of said washing solution no less than three times the volume of said non-valved conduit(s), and used washing solution within said SOP-forming tank is expelled via said outlet ports into said non-valved conduit(s), then transferred as per step (c) using pumps;
e) cleaning said non-valved conduit(s) between said SOP-forming tank and said SOP
separator after completion of step (d) with said washing solution wherein cleaning is done with a volume of said washing solution no less than three times the volume of said non-valved conduit(s), and used washing solution introduced into said non-valved conduit(s) is transferred as per step (c) using pumps;
f) disconnecting said non-valved conduit(s) from said at least one inlet, then flushing said SOP-forming tank and said non-valved conduit(s) between said SOP-forming tank and said SOP separator after completion of step (e) with liquid water having a temperature below the boiling point until clear water flows freely from the disconnected end of said non-valved conduit(s).
a) producing a uniformly dispersed suspension by continuously stirring or mixing said fluid suspension within said SOP-forming tank until such time as said fluid suspension has been expelled from said SCP-forming tank via said outlet ports into said non-valved conduit(s) leading to at least one inlet;
b) expelling to the fullest extent possible all uniformly dispersed suspension of said fluid suspension produced in step (a) within said SOP-forming tank from said SOP-forming tank via said outlet ports into said non-valved conduit(s), using pumps;
c) transferring the uniformly dispersed suspension of said fluid suspension via said non-valved conduit(s) to and through said at least one inlet into said SOP
separator using pumps;
d) washing the walls of said SOP-forming tank thoroughly after completion of step (b) with a washing solution wherein washing is done with a volume of said washing solution no less than three times the volume of said non-valved conduit(s), and used washing solution within said SOP-forming tank is expelled via said outlet ports into said non-valved conduit(s), then transferred as per step (c) using pumps;
e) cleaning said non-valved conduit(s) between said SOP-forming tank and said SOP
separator after completion of step (d) with said washing solution wherein cleaning is done with a volume of said washing solution no less than three times the volume of said non-valved conduit(s), and used washing solution introduced into said non-valved conduit(s) is transferred as per step (c) using pumps;
f) disconnecting said non-valved conduit(s) from said at least one inlet, then flushing said SOP-forming tank and said non-valved conduit(s) between said SOP-forming tank and said SOP separator after completion of step (e) with liquid water having a temperature below the boiling point until clear water flows freely from the disconnected end of said non-valved conduit(s).
31. The process of Claim 28 wherein the cake of washed, bleached, rinsed and partially dehydrated SOP and the filter are physically removed from said SOP separator following completion of processing.
32. The process of Claim 29 wherein the cake of washed and partially dehydrated SOP and the filter are physically removed from said SOP separator following completion of processing.
33. The process of Claim 19, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, the clear liquid expelled from outlet(s) of said SOP separator, distillation of said clear liquid and condensation of the distillate produced from said clear liquid, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
34. The process of Claim 20, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, the clear liquid expelled from outlet(s) of said centrifuge, distillation of said clear liquid and condensation of the distillate produced from said clear liquid, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
35. The process of Claim 21, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, the clear liquid expelled from outlet(s) of said clothes washing machine, distillation of said clear liquid and condensation of the distillate produced from said clear liquid, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
36. The process of Claim 22, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, a clear liquid expelled from outlet(s) of said positive pressure filtration system, distillation of said clear liquid and condensation of the distillate produced from said clear liquid, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
37. The process of Claim 23, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, a clear liquid expelled from outlet(s) of said vacuum filtration system, distillation of said clear liquid and condensation of the distillate produced from said clear liquid, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
38. The process of Claim 24, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, a clear liquid expelled from outlet(s) of said gravity-flow filtration system, distillation of said clear liquid and condensation of the distillate produced from said clear liquid, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
39. The process of Claim 28, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, said used washing solution, said used bleaching solution, said used rinsing solution and said used dehydration alcohol, distillation of said used washing solution, used bleaching solution, used rinsing solution and used dehydration alcohol and condensation of the distillate produced from said used washing solution, used bleaching solution, used rinsing solution and used dehydration alcohol, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
40. The process of Claim 29, further comprising the steps of transferring from the storage container to a distillation apparatus via conduit(s), using pumps and valves, said used washing solution and said used dehydration alcohol, distillation of said used washing solution and used dehydration alcohol and condensation of the distillate produced from said used washing solution and used dehydration alcohol, and transfer of said distillate to an alcohol storage tank via conduit(s), using pumps and valves, leaving a residue of non-distilled aqueous solution in said distillation apparatus.
41. The process of any one of Claims 33, 34, 35, 36, 37, 38, 39, or 40 wherein said distillation apparatus operates to provide vapour at or near the boiling point of an aliphatic alcohol.
42. The process of any one of Claims 33, 34, 35, 36,-,37, 38, 39, or 40 wherein said distillation apparatus operates under reduced pressure to produce vapour below the boiling point of an aliphatic alcohol.
43. The process of any one of Claims 33, 34, 35, 36, 37, 38, 39, or 40 wherein said conduit(s), pumps and valves are physically and chemically compatible with an used alcohol-containing solutions.
44. The process of any one of Claims 33, 34, 35, 36, 37, 38, 39, or 40 further comprising recovery of alkaline hydroxide as alkaline soaking solution and recycling of said alkaline soaking solution to an extraction vessel following completion of the following steps:
a) transferring a known volume of said residue of non-distilled aqueous solution from said distillation apparatus via conduit(s), using pumps and valves, to an alkali storage tank to stir and / or mix its contents;
b) titrating said residue of non-distilled aqueous solution in said alkali storage tank to determine the alkalinity of said residue of non-distilled aqueous solution;
c) adding a required mass of alkali to said alkali storage tank followed by stirring and /or mixing to produce alkaline soaking solution;
d) transferring alkaline soaking solution produced in step (c) to an extraction vessel when required.
a) transferring a known volume of said residue of non-distilled aqueous solution from said distillation apparatus via conduit(s), using pumps and valves, to an alkali storage tank to stir and / or mix its contents;
b) titrating said residue of non-distilled aqueous solution in said alkali storage tank to determine the alkalinity of said residue of non-distilled aqueous solution;
c) adding a required mass of alkali to said alkali storage tank followed by stirring and /or mixing to produce alkaline soaking solution;
d) transferring alkaline soaking solution produced in step (c) to an extraction vessel when required.
45. The process of any one of Claims 33, 34, 35, 36, 37, 38, 39, or 40 further comprising cleaning of said distillation apparatus and comprising the steps of:
a) transferring said residue of non-distilled aqueous solution from said distillation apparatus via conduit(s), using pumps and valves, to an alkali storage tank;
b) removing solids remaining in said distillation apparatus by physical means;
c) removing any residue of solids remaining in said distillation apparatus following step (b) by dissolving the residue of solids and removing the solution.
a) transferring said residue of non-distilled aqueous solution from said distillation apparatus via conduit(s), using pumps and valves, to an alkali storage tank;
b) removing solids remaining in said distillation apparatus by physical means;
c) removing any residue of solids remaining in said distillation apparatus following step (b) by dissolving the residue of solids and removing the solution.
46. The process of any one of Claims 33, 34, 35, 36, 37, 38, 39 or 40 wherein said residue of non-distilled aqueous solution was derived from plant tissues.
47. The process of any one of Claims 33, 34, 35, 36, 37, or 38 wherein said residue of non-distilled aqueous solution when present was derived from said clear liquid expelled from outlet(s) of said SOP separator and/ or said centrifuge and/or said clothes washing machine and/or said positive pressure filtration system and/or said vacuum filtration system and/or said gravity-flow filtration system.
48. The process of Claim 39 and/or Claim 40 wherein the residue of non-distilled aqueous solution when present was derived exclusively from said used washing solution.
49. The process of Claim 39 wherein the residue of non-distilled aqueous solution when present was derived exclusively from said used bleaching solution.
50. The process of Claim 39 wherein the residue of non-distilled aqueous solution when present was derived exclusively from said used rinsing solution.
51. The process of Claim 39 and/or Claim 40 wherein the non-distilled aqueous solution when present was derived exclusively from said used dehydration alcohol.
52. A process to produce a clear solution of water miscible oligosaccharides and polysaccharides (MOP) from a cake of solid oligosaccharides and polysaccharides (SOP) comprising the steps of:
a) weighing a mass of said cake of SOP;
b) adding to said mass a volume in litres of water equaling at least twice the mass in kilograms of said cake of SOP;
c) mixing together said cake of SOP and said water at a temperature between 0 °C and 100 °C until a clear solution is obtained.
a) weighing a mass of said cake of SOP;
b) adding to said mass a volume in litres of water equaling at least twice the mass in kilograms of said cake of SOP;
c) mixing together said cake of SOP and said water at a temperature between 0 °C and 100 °C until a clear solution is obtained.
53. A mixture of water soluble and/or miscible solid oligosaccharides and polysaccharides (SOP) obtained as cakes of dehydrated primary SOP as formed by any one of the processes of Claims 1, 19, 29 and 32.
54. A mixture of water soluble and/or miscible solid oligosaccharides and polysaccharides (SOP) obtained as cakes of bleached dehydrated primary SOP by any one of the processes of Claims 1, 28 and 31.
55. A mixture of water soluble and/or miscible solid oligosaccharides and polysaccharides (SOP) obtained as cakes of dehydrated secondary SOP by any one of the processes of Claims 18, 19, 29 and 32.
56. A mixture of water soluble and/ or miscible solid oligosaccharides and polysaccharides (SOP) obtained as cakes of bleached dehydrated secondary SOP by any one of the processes of Claims 28 and 31.
57. A clear aqueous solution of miscible oligosaccharides and polysaccharides (MOP) obtained from said dehydrated primary SOP of Claim 53 via the process of Claim 52.
58. A clear aqueous solution of miscible oligosaccharides and polysaccharides (MOP) obtained from said bleached dehydrated primary SOP of Claim 54 via the process of Claim 52.
59. A clear aqueous solution of miscible oligosaccharides and polysaccharides (MOP) obtained from said dehydrated secondary SOP of Claim 55 via the process of Claim 52.
60. A clear aqueous solution of miscible oligosaccharides and polysaccharides (MOP) obtained from said bleached dehydrated secondary SOP of Claim 56 via the process of Claim 52.
Priority Applications (1)
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CA2675940A CA2675940C (en) | 2009-08-10 | 2009-08-10 | Basic sop process for recovery of oligosaccharides and polysaccharides from plants |
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CA2675940A CA2675940C (en) | 2009-08-10 | 2009-08-10 | Basic sop process for recovery of oligosaccharides and polysaccharides from plants |
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CA2675940A1 CA2675940A1 (en) | 2011-02-10 |
CA2675940C true CA2675940C (en) | 2013-07-23 |
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CA2675940A Expired - Fee Related CA2675940C (en) | 2009-08-10 | 2009-08-10 | Basic sop process for recovery of oligosaccharides and polysaccharides from plants |
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