WO2006125286A1 - Procede de production de dextrose cristalline anhydre sans pyrogene a haute purete a partir du saccharose - Google Patents

Procede de production de dextrose cristalline anhydre sans pyrogene a haute purete a partir du saccharose Download PDF

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Publication number
WO2006125286A1
WO2006125286A1 PCT/BR2005/000092 BR2005000092W WO2006125286A1 WO 2006125286 A1 WO2006125286 A1 WO 2006125286A1 BR 2005000092 W BR2005000092 W BR 2005000092W WO 2006125286 A1 WO2006125286 A1 WO 2006125286A1
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WO
WIPO (PCT)
Prior art keywords
fact
solution
weight
process according
concentration
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Application number
PCT/BR2005/000092
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English (en)
Inventor
João Afonso FERREIRA
Cláudio Octávio TEIXEIRA
Sérgio Murilo SOARES
Original Assignee
Getec Guanabara Química Industrial S.A.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Getec Guanabara Química Industrial S.A. filed Critical Getec Guanabara Química Industrial S.A.
Priority to BRPI0520266-3A priority Critical patent/BRPI0520266B1/pt
Priority to PCT/BR2005/000092 priority patent/WO2006125286A1/fr
Publication of WO2006125286A1 publication Critical patent/WO2006125286A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/005—Purification of sugar juices using chemicals not provided for in groups C13B20/02 - C13B20/14
    • 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
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/002—Purification of sugar juices using microorganisms or enzymes
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/12—Purification of sugar juices using adsorption agents, e.g. active carbon
    • C13B20/123—Inorganic agents, e.g. active carbon
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups

Definitions

  • the present invention relates to a process for the production of anhydrous crystalline dextrose of high chemical purity and free of pyrogen through crystallization thereof, which is accomplished by the controlled evaporation of an aqueous solution of glucose, said glucose being obtained from sugar cane sucrose.
  • the said dextrose, prepared by the process in accordance with the invention is composed of well-defined crystals, and is constituted of particles which exhibit a narrow size distribution with a mean diameter comprised between about 100 microns and about 400 microns.
  • the physical and functional characteristics of the anhydrous crystalline dextrose according to the invention are carefully adjusted in order to maximize its performance in applications in the food and pharmaceutical industries.
  • the technical field of the invention is concerned with naturally occurring nutritive sweeteners, the most important of these being the sucrose, the glucose and the fructose, which are saccharides produced on a large industrial scale and widely consumed as simple sugars and as ingredients in various edible products.
  • Dextrose also known as glucose
  • Dextrose is an aldohexose having the molecular formula C 6 H ⁇ Oe and a molecular weight of 180.2, broadly belonging to the class of pyranoses, and exhibiting a sweetening power approximately equivalent to 70% that of sucrose, when used on an equivalent weight basis.
  • the crystalline form of this important monosaccharide is composed of orthorhombic crystals which are white, odorless and have a sweet taste; said crystals have an apparent density higher than 740 kg/m 3 and a melting point of 146 °C, and are sparingly soluble in ethanol and highly soluble in water.
  • the French patent FR 2,595,715 describes a process for preparing dextrose using the sucrose as raw material.
  • the said process despite stating in its description the possibility of obtaining anhydrous dextrose, reveals only the manufacture of monohydrate dextrose in its experimental exemplifications.
  • This said process comprises, after an initial phase of inversion of sugar, i.e. its transformation into a solution of glucose and fructose, chromatographic separation unit operations, with the reuse of the fructose stream by means of its enzymatic isomerization, purification, concentration, crystallization and centrifugation .
  • the present invention embraces distinguishing characteristics in introducing a technology which is distinct from those of the prior art, by combining the sugar cane sucrose as the source of raw material and an integrated processing route which is original and economical for producing the pyrogen-free anhydrous dextrose.
  • the present patent application exhibits several features that are significantly different from those of all the other processes revealed in the literature of the prior art, possessing a high degree of inventiveness.
  • inventiveness besides embodying a focus on the production of a dextrose that is simultaneously anhydrous and free of pyrogen, is unique owing to its various technical improvements and innovations that combine to form a simple and effective processing route which comprises the following steps:
  • step (b) chemical hydrolysis of the sucrose solution resulting from step (a) by employing an acid selected from the group consisting of inorganic acids, having the pH controlled in the range of
  • step (c) neutralization of the solution resulting from step (b) with sodium hydroxide, followed by its deionization at a temperature lower than 50 0 C;
  • step (d) chromatographic fractionation of the solution of glucose and fructose carried out at a temperature of the feed to the column in the range of 58 0 C to 62 0 C;
  • step (i) crystallization of the dextrose from the syrup resulting from step (h) ;
  • sucrose is of fundamental importance to the success of the subsequent operations employed in the production of dextrose.
  • the commercially available sucrose is usually contaminated with starch with various concentrations.
  • sucrose is processed directly without the previous elimination of this residual starch, the preparation of the final product will be harmed due to the formation of several contaminants that interfere with the dextrose crystallization. In the execution of the industrial process, these contaminants impair the quality of the finished product and the process yield, and may even completely inhibit the crystallization of the final product.
  • the anhydrous dextrose produced by the process in accordance with the invention has a high degree of purity, which is quantified by glucose content higher than 99.70%.
  • the raw material which combines, advantageously, the strategic and commercial characteristics and allows the establishment of a technological route which is more simple, efficient and productive, thereby meeting all the criteria specified in the inventive concept is the sucrose obtained from the sugar cane.
  • the sucrose from sugar cane is a feedstock which is available on a large scale, is subject to few seasonal fluctuations in its demand, supplied regularly with a good product quality by a great number of producers and, furthermore, it has been historically cheaper than starchy raw materials.
  • Figure 1 shows schematically the process for the manufacture of pyrogen-free anhydrous crystalline dextrose of high purity from sucrose.
  • the crystalline sucrose received from the suppliers with a minimum purity of 99.5% by weight, on a dry solids basis, is dissolved in process water, thereby forming an aqueous solution having a concentration of about 60% by weight, and is then subjected to an essential and innovative enzymatic treatment accomplished with an amylase, for about 45 minutes at a mean temperature of between 78 °C and 82 0 C, preferably at 80 0 C, said treatment not being found in the technical documents of the prior art, aiming at the convenient elimination of any residual starch that may exist in the medium and that could seriously hinder the filterability of the final product.
  • this sucrose solution after occasional impurities have been removed by means of a filtration operation using a filter aid, undergoes a hydrolysis reaction catalyzed by hydrochloric acid, or by another inorganic acid, which is added as an aqueous solution in order to maintain the pH within the range of 1.9 to 2.1, thereby resulting a solution of fructose and glucose having a dry solids concentration of between 58% and 62% by weight, preferably of 60% by weight, and a maximum admissible glucose content of 1.5% by weight.
  • the resultant solution is neutralized with sodium hydroxide and purified by deionization, at a temperature never higher than 50 0 C, in an ion exchange unit whose purpose is the removal of all the cations and anions that could contaminate, in the subsequent step, the resin which constitutes the packing material of a chromatographic separation column, which forms an integral part of the process, what would cause a significant reduction in the level of performance of the column operation.
  • the partial separation of the glucose from the fructose takes place, where the glucose-enriched fraction is concentrated in order to obtain a glucose-rich syrup, which also contains minute amounts of fructose.
  • the aqueous solution of fructose and glucose having a dry solids concentration comprised between 58% and 59% by weight, obtained previously just after the deionization operation, and at a temperature comprised between 58 0 C and 62 0 C is fed into a chromatographic column containing a packed bed formed by a cation-exchange resin which adsorbs the fructose to a greater degree than it adsorbs the glucose, thereby resulting, as a consequence of this selective retention of the fructose in the resin, a partial fractionation of these two isomers.
  • a certain volume of elution water which has been deoxygenated and deionized in a special ion exchange unit, is introduced into the chromatographic column to effect the desorption of fructose from the resin, thereby forming a fructose stream with a dry solids concentration comprised between 22% and 26% by weight, and having a fructose content comprised between 84% and 90% by weight, on a dry solids basis, preferably comprised between 86% and 88% by weight, and which stream is employed in the production of sorbitol in association with mannitol, such compounds being polyols which have a wide range of industrial uses, and, moreover, a glucose stream, said stream being the main focus of the present invention, having a dry solids concentration of between 22% and 26% by weight, and a glucose content of between 94% and 97% by weight, on a dry solids basis, preferably of greater than 95.5% by weight, on the dry basis, thereby allowing the formation of dext
  • This glucose solution whose temperature is adjusted to a value within the range of 57 0 C to 61 0 C, preferably within the range of 58 0 C to 60 0 C, and having a pH of about 3.5, is then subjected to a treatment with active charcoal in an approximate proportion of between 0.1% and 0.3% wt/vol, preferably of between 0.1% and 0.2% wt/vol, for about 45 minutes, in order to remove color from the product, after which there is accomplished the filtration of the stream using a filter aid to separate both the charcoal and the impurities adhered to its surface.
  • the glucose syrup which has already been cooled so that it does not reach a temperature higher than the limit of 50 °C, is fed into a battery of decolorizing, cationic and anionic beds wherein it is clarified and deionized until its color and resistivity satisfy entirely the requirements represented by the predefined process parameters.
  • the stream is subjected to a second treatment with active charcoal, said charcoal having smaller particle sizes and higher specific surface area when compared to the first one, in the approximate proportion of between 0.1% and 0.3% wt/vol, preferably of between 0.1% and 0.2% wt/vol, at a temperature adjusted within the range of 65 °C to 70 0 C, and having the pH adjusted in the range of 3.0 to 4.0, preferably in the range of 3.3 to 3.6, followed by the filtration of the solution employing a filter aid so as to remove the charcoal and all the impurities adsorbed on it.
  • the syrup passes through a battery of low-porosity filters in series, before being concentrated to the content levels required in the crystallization cycles.
  • the solution is fed into a multiple-effect evaporator so that its concentration is increased from the initial range of 22% to 26% by weight until it reaches the final condition considered to be ideal for storage in the crystallizer, more specifically in the range of 76% to 80% by weight, preferably in the range of 78% to 80% by weight.
  • the final steps in the sequence of the process operations in accordance with the present invention comprise the crystallization of the anhydrous dextrose, the recovery of the dextrose crystals through the centrifugation of the massecuite, and the washing and drying of such crystals.
  • This crystallization of anhydrous dextrose said crystallization being a central point in this last series of operations, has its success heavily dependent on the previous unit operations, especially those concerned with the purification of the glucose solution, inasmuch as the shape, the size and the granulometric characteristics of the crystals thus generated are factors which are greatly influenced by contaminants that exist in the aqueous medium where the appearance and the growth of the crystal nuclei take place.
  • the crystallization of the glucose by the evaporation of its syrup is then initiated by storing the product obtained in the preceding phase, with a concentration being preferably in the range of 78% to 80% by weight and at a temperature of between 60 0 C and 63 0 C.
  • a concentration being preferably in the range of 78% to 80% by weight and at a temperature of between 60 0 C and 63 0 C.
  • the medium is subjected to a controlled heating that results in an hourly elevation of the concentration in the range of 0.8% to 1.0%, thereby causing this variable to reach the predefined level of between 81% and 82% by weight.
  • the crystals are separated by centrifugation, washed with process water at a temperature in the range of 60 0 C to 65 °C and discharged from the automatic centrifuges as a cake having a moisture content of between 1% and 5%, preferably between 2% and 3%, whereas the mother liquor is used directly as raw material for the associated production of sorbitol, after having been conveniently hydrogenated.
  • the moist crystals are then transferred to the drying system and brought into contact with an air stream which has been filtered through absolute filters and preheated to a temperature in the range of 125 °C to 135 0 C, there being important to point out that, during the course of this operation, the product temperature is monitored so as not to exceed the upper limit of 45 0 C, otherwise a degradation of the dextrose could occur.
  • the mass of crystals is screened for the separation of occasional agglomerates and, finally, after having been weighed, it is packed into adequate containers in order to be transported to the economic market.
  • the crystallization step exhibits yields of recovery of anhydrous dextrose in the crystalline form, based on the mass of dextrose contained in the feed syrup, comprised between about 40% and about 44%, preferably comprised between 42% and 43%, said yields demonstrating the great efficiency of this novel technology.
  • the purity of the crystals produced by the process in question is excellent, being manifested by a content of glucose always higher than 99.70% by weight, on a dry solids basis, and a content of fructose, which is virtually the sole residual impurity in the crystalline product, lower than 0.30% by weight, on a dry solids basis.
  • these microcrystalline particles exhibit a considerably narrow granulometric distribution with a mean diameter comprised between about 100 microns and about 400 microns, and possess a residual moisture content lower than the predetermined upper limit of 0.5% by weight.
  • the technical specifications of the final product obtained, particularly its chemical purity meet all the international standards for the anhydrous crystalline dextrose required by the market.
  • this invention by choosing the sucrose obtained from sugar cane and by innovating the technological route for the production of anhydrous crystalline dextrose, constitutes an industrial alternative which makes it possible to achieve a combination of strategic, technical, economic, and commercial factors which is distinctly different from and much better than those employed by the prior art. Furthermore, the technical novelties and improvements incorporated into the process in accordance with the invention give rise to important technical effects, of which stand out the elimination of the residual starch contained in the sucrose and the purification of the glucose solution in order to render it free from pyrogen, thereby becoming relevant, with the purpose of providing a better understanding of its component phases, to illustrate it by means of the following preparation example, which does not limit the scope thereof.
  • sucrose having a purity of 99.8% by weight, on a dry solids basis, and a dry solids concentration of 59% by weight, was subjected to a purification treatment with an amylase-type enzyme to remove the residual starch, for 44 minutes and at a temperature of 81°C; thereafter, this sucrose, which had already been filtered, underwent a hydrolysis catalyzed by an aqueous solution of hydrochloric acid having a pH equivalent to 2.1, thereby forming a solution of fructose and glucose, also known as invert sugar, and still having a dry solids concentration of 59% by weight and a sucrose content of 0.8%.
  • the said solution of fructose and glucose having already been neutralized and deionized, was then fed into a chromatographic separation column, with a dry solids concentration of 58% by weight and at a temperature of 59 °C.
  • elution water which had been previously deoxygenated and deionized in an ancillary system, was introduced into the chromatographic column, thereby effecting the desorption of fructose from the resin, in order to permit, as a consequence, the formation of a main solution of fructose and glucose having a concentration of 24% by weight and a glucose content of 96% by weight, on a dry solids basis, in addition to another stream, which stream does not belong to the focus of interest of the present invention, with a broadly similar concentration and a fructose content of about 87% by weight, on the dry basis.
  • the aforesaid glucose-rich solution whose temperature was maintained at 60 0 C, and at a pH equivalent to 3.6, was subjected to a first treatment with active charcoal in the exact proportion of 0.1% wt/vol for 40 minutes, followed by the filtration of the stream to remove the charcoal and the impurities adsorbed on it and, after accomplishing the cooling of the stream to 44 °C, to the deionization of the syrup carried out in decolorizing, cationic and anionic beds .
  • the said glucose solution with the specific aim of removing any occasional pyrogen that might have been carried by it, was subjected to a second treatment with active charcoal, in the same proportion of 0.1% wt/vol, at a temperature of 68 0 C and having the pH adjusted to the value of 3.5, followed by a filtration operation to separate the charcoal and the impurities adsorbed on it.
  • the glucose syrup which had been exhaustively purified was fed into a triple-effect evaporation unit, wherein its dry solids concentration increased to the level of 78%.
  • the medium had its dry solids concentration raised at a rate of 1.0% an hour, until it attained a value of 81%. After having been accomplished the seeding of the medium, its concentration was raised once again, but now at a rate of 0.4% an hour, under the same vacuum, thereby attaining a content of crystals of 42% at the exact point when its concentration reached a value of 88%.
  • the recovery of the dextrose crystals was effected by means of centrifugation of the massecuite, followed by the washing of the said crystals in the automatic centrifuge proper, with process water at a temperature of 60 0 C, and subsequently by the drying through direct contact with dry air at a temperature of 130 0 C.
  • the material obtained attained a final moisture content of 0.4% by weight, and was then ready to be screened and packed in an environment with controlled conditions.
  • the anhydrous crystalline dextrose of high purity and free of pyrogen produced by the process according to the invention exhibited a glucose content of 99.85% by weight, on a dry solids basis, a fructose content of 0.15% by weight, on a dry solids basis, a mean diameter of 290 microns, and a granulometric distribution with about 80% of its particles comprised in the range of 100 to 400 microns, in consonance with the market demand.

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Abstract

L'invention concerne un procédé de production de dextrose cristalline anhydre d'une haute pureté chimique et dépourvu de pyrogène en utilisant le saccharose de la canne à sucre comme matière première. Ce procédé produit des particules microcristallines bien définies morphologiquement, ces particules étant caractéristiques du système cristallin orthorhombique et présentant une composition granulométrique étroite présentant un diamètre moyen compris entre 100 et 400 microns.
PCT/BR2005/000092 2005-05-24 2005-05-24 Procede de production de dextrose cristalline anhydre sans pyrogene a haute purete a partir du saccharose WO2006125286A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
BRPI0520266-3A BRPI0520266B1 (pt) 2005-05-24 2005-05-24 Processo de produção de dextrose cristalina anidra de elevada pureza e livre de pirogênio a partir de sacarose
PCT/BR2005/000092 WO2006125286A1 (fr) 2005-05-24 2005-05-24 Procede de production de dextrose cristalline anhydre sans pyrogene a haute purete a partir du saccharose

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/BR2005/000092 WO2006125286A1 (fr) 2005-05-24 2005-05-24 Procede de production de dextrose cristalline anhydre sans pyrogene a haute purete a partir du saccharose

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WO2006125286A1 true WO2006125286A1 (fr) 2006-11-30

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101205561B (zh) * 2006-12-20 2010-10-06 凯能高科技工程（上海）有限公司 葡萄糖结晶母液回收工艺
WO2014030030A1 (fr) * 2012-08-20 2014-02-27 Naturalia Ingredients S.R.L. Procédé de production de produit contenant du sucre à partir d'un fruit
CN108251470A (zh) * 2017-11-03 2018-07-06 毛强平 一种果葡糖浆的制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1133046A (en) * 1966-03-03 1968-11-06 Colonial Sugar Refining Co Treatment of sugar solutions
US5837060A (en) * 1994-02-15 1998-11-17 Roquette Freres Process for the manufacture of a starch hydrolysate of low polymolecularity index, obtention and use of novel starch hydrolysate in peritoneal dialysis
US20040231662A1 (en) * 2001-08-15 2004-11-25 De Mendonca Ferreira Joao Afonso Process for the production of crystallin fructose of high purity utlizing fructose syrup having a low content of fructose made from sucrose and product obrained

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1133046A (en) * 1966-03-03 1968-11-06 Colonial Sugar Refining Co Treatment of sugar solutions
US5837060A (en) * 1994-02-15 1998-11-17 Roquette Freres Process for the manufacture of a starch hydrolysate of low polymolecularity index, obtention and use of novel starch hydrolysate in peritoneal dialysis
US20040231662A1 (en) * 2001-08-15 2004-11-25 De Mendonca Ferreira Joao Afonso Process for the production of crystallin fructose of high purity utlizing fructose syrup having a low content of fructose made from sucrose and product obrained

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SCHORMUELLER J. ET AL.: "Handbuch der Lebensmittelchemie", vol. BAND V/1, 1967, BERLIN: SPRINGER VERLAG, article GRAEFE G.: "B. Glucosesirup (Staerkesirup),Staerkezucker und Dextrose (Traubenzucker)", pages: 637 - 665, XP008074024 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101205561B (zh) * 2006-12-20 2010-10-06 凯能高科技工程（上海）有限公司 葡萄糖结晶母液回收工艺
WO2014030030A1 (fr) * 2012-08-20 2014-02-27 Naturalia Ingredients S.R.L. Procédé de production de produit contenant du sucre à partir d'un fruit
CN104837376A (zh) * 2012-08-20 2015-08-12 天然成分有限责任公司 从水果中制备糖产品的方法
JP2015527356A (ja) * 2012-08-20 2015-09-17 ナチュラリア イングリーディエンツ ソシエタ レスポンサビリタ リミタータＮＡＴＵＲＡＬＩＡ ＩＮＧＲＥＤＩＥＮＴＳ Ｓ．ｒ．ｌ． 果物から砂糖製品を製造する方法
CN108251470A (zh) * 2017-11-03 2018-07-06 毛强平 一种果葡糖浆的制备方法

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