US3929503A - Production of free-flowing particles of glucose, fructose or the mixture thereof - Google Patents

Production of free-flowing particles of glucose, fructose or the mixture thereof Download PDF

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Publication number
US3929503A
US3929503A US475198A US47519874A US3929503A US 3929503 A US3929503 A US 3929503A US 475198 A US475198 A US 475198A US 47519874 A US47519874 A US 47519874A US 3929503 A US3929503 A US 3929503A
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Prior art keywords
sugar
fructose
glucose
particles
powder
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Expired - Lifetime
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US475198A
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English (en)
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Toshio Yamauchi
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Daiichi Pharmaceutical Co Ltd
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Daiichi Pharmaceutical Co Ltd
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    • 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
    • C13K1/10—Crystallisation

Definitions

  • aqueous solutions containing glucose, fructose or mixtures thereof are converted into the form of dry powders, pellets, granules or the like without subjecting the-solution to a crystallization step.
  • Fructose or mixtures thereof with glucose are widely consumed in the form of a dry powder or solution. Although anhydrous crystalline fructose has been used even for dietary purposes, it is not essential that the fructose used for such purposes be pure, but rather a supply of fructose as cheap as possible in large quantities is more important when its nutritional value is taken into consideration. Fructose can also be produced from glucose by the action of the enzyme glucose isomerase. At equilibrium, the reaction mixture contains 43% fructose and 57% glucose but is very hygroscopic and difficult to crystallize. Therefore, the isomerized products are used as sweeteners for confectionaries and other food products in the form of a syrup.
  • the syrup has certain disadvantages in that it is susceptible to deterioration due to coloration, microorganism growth or partial crystallization in winter on storage. It is, therefore, desirable to convert the syrup to a free-flowing solid which may find wide use in various fields, particularly in houshold consumption.
  • fructose solutions having at least a 95% concentration are further concentrated in vacuo to a water content from 2 to 5%, and then cooled to from 60 to 85C.
  • a large quantity of fructose crystals is added to the solution and the mixture is stirred at a temperature of 60 to 85C until it becomes a soft mass.
  • the mass is made solid, ground and dried at a temperature below 65C.
  • This method has the difficulty of concentrating fructose to a concentration higher than 95%.
  • An object of the present invention is to provide an economical method of producing free-flowing, anhydrous particles of glucose, fructose or mixtures thereof in such forms as powders, pellets, granules and the like.
  • Another object is to provide a method whereby aqueous solutions of glucose, fructose or mixtures thereof are converted into dry, free-flowing particles such as powders, pellets granules and the like without subjecting the. solution to a crystallization step.
  • crystals or powder of anhydrous glucose, fructose or mixtures thereof (hereinafter referred to as mother powder) are mixed and kneaded with a syrup or massecuite (hereinafter referred as syrup) containing 40 to 90%, preferably 60 to 90% of the same type of sugar as the mother powder so that the mixture forms wet particles having a moisture content of less than 7%, preferably from 1.5 to 4%.
  • This step may be conveniently carried out by charging the mother powder in a kneader and adding the syrup gradually to the mother powder in amounts sufficient to make the moisture content less than 7%.
  • the mother powder and the syrup may be mixed continuously by supplying them at a constant rate to a continuous mixer. This mixing may be carried out at room temperature or higher. Thus, hot syrup just withdrawn from a vacuum evaporator (about C) can be mixed without cooling. During this mixing step, the mixture forms wet, round fine particles which are still free-flowing. At this stage, the mixture may easily be shaped into a suitable size of granules or pellets using a conventional type of granulator or pelletizer. The wet granules or pellets are then dried.
  • the wet particles may be dried without subjecting them to a granulating or pelletizing ste 'l he resulting particles, granules or pellets are dried at a temperature below 70C, preferably at about 60C, under reduced pressure, for example at 10mm Hg.
  • Other drying methods such as air-blowing or fluid drying may also be applied.
  • air is preferably dehumidified to an absolute humidity less than about 0.0lg of water per g. of air and heated from 50C to 70C.
  • the resulting products are free-flowing particles or pellets having an average particle size from 0.05 to 0.3mm.
  • the granules preferably have a cylindrical form of 0.5 to 1.5mm in diameter and about 2mm in length.
  • the finished products are generally uniform in shape and size, it is sometimes desirable to sieve the product through a screen.
  • the mixture of the mother powder and the syrup has a moisture content less than 7%.
  • the mixture is a mud which turns into an aqueous solution of sugar on heating during the subsequent drying step. Thus, drying into solid particles becomes impossible.
  • the concentration of syrup is represented on the horizontal axis and the ratio of the weight of syrup to the weight of mother powder is represented in the vertical axis.
  • Curve AB represents this ratio at varying concentrations of syrup to give a 7% moisture content
  • curves A B and C D are those of 4% and 1.5% moisture contents respectively.
  • the present invention is carried out within the range defined by points A, B, C and D, preferably the range defined points A, B, C, and D in the drawing.
  • the weight of mother powder Wp, the weight of syrup Ws and the percentage of water content in the syrup Xs are in the relationship represented by the following equations: Ws Xs/Wp Ws 7, or preferably, 1.5 Ws Xs/Wp+Ws 4 out at a sugar concentration of syrup between 40% and 95%.
  • the mother powder must be used in a very large quantity.
  • the sugar concentration is preferably from 40 to 90% by weight of glucose, fructose or a mixture thereof.
  • the ratio of the quantities of the syrup to the mother powder, the sugar concentration of the syrup and the moisture content of the mixture of the mother powder with the syrup are less than 130% by weight, less than 95% by weight and less than 7% by weight, perferably to 65% by weight, 40 to 90% by weight and 1.5 to 4% by weight respectively.
  • binders such as carboxymethylcellulose or sodium alginate, and/or lubricants such as sugar ester with higher alkanoic acid may be used.
  • the syrup not only aqueous solutions of glucose, fructose or mixtures thereof but also the corresponding massecuite may be used. In the latter case, 30 to 50% of the total sugar must be present in the form of crystals and the quantity thereof should be included in the quantity of the mother powder.
  • Other examples of the syrup are green syrup separated from the massecuite as mentioned (sugar concentration 80 to 90%), or syrup produced by the isomerization of glucose with ion-exchanger or enzyme followed by concentrating to a concentration from 70 to 90%. Invert sugar made from sucrose may also be employed.
  • the starting mother powder may be anhydrous crystals of the same type of sugar as mentioned.
  • the particle size of the crystals is preferably 0.005 to 0.3mm.
  • the finished product which is substantially free from water is advantageously used as the mother powder in the subsequent cycle of the operation.
  • the sugar need not always be the same in the syrup and the mother powder used.
  • the syrup obtained invention .mercially available isomerized glucose solution with pure anhydrous fructose crystals.
  • the method of the present invention may preferably be practiced by returning a part of the finished product corresponding to the amount of mother powder used in the previous cycle to the subsequent cycle as the mother powder therefor.
  • This recycling of mother powder can be conducted either in batch type or continuous operation.
  • the finished product may be withdrawn from each cycle of the operation in an amount corresponding to the sugar content of the syrup.
  • sugar is not deteriorated because the drying is carried out at a temperature below C.
  • EXAMPLE 1 charged in the kneader. 0.8 kg of an 83.8% aqueous solution of sugar consisting of 98.7% of fructose and 1.3% of glucose was added to the powder. After 10 to 15 minutes kneading, the resulting mixture became wet, free-flowing aggloinerates of crystals. The mixture retained 2.79% of water and the purity of fructose therein was 99.7%. The mixture was granulated by extruding through a screen at room temperature, and the granules were dried in a vacuum chamber at lOmm Hg and 65C for 4 hours. Free-flowing granules having a moisture content of 0.10% and an apparent density of 0.53 g/ml were obtained.
  • EXAMPLE 2 parts by weight of dried granules obtained in I Example 1 was mixed with 38 parts by weight of anhydrous glucose.
  • the mixture was pulverized to fine particles of 50 mesh (Tyler).
  • 4.0 kg of the resulting powder (moisture content 0.25%) was kneaded as in Example 1 with 1.55 kg of the same syrup as used in Example 1.
  • the resulting mixture having' a moisture content of 3.0% was pelletized to small pellets using a laboratory type rotary disc-pelletizer at room temperature.
  • the 7 resulting freefflowingwet pellets were dried as in Example l. Free-flowing pellets having moisture content of 0.17 and an apparent density of 0.59 g/ml were obtained.
  • EXAMPLE 3 In this example, the mother powder and the syrup were continuously mixed using a double screw type continuous mixer.
  • the same type of sugar powder as used in Example 2 (particle size less than 50am, moisture content 0.19%) and a 12.2% solution of isomerized glucose (fructose 70%, glucose 30%) were supplied at a ratio 4:0.76 parts by weight.
  • the mixture passed through the mixer for about 15 minutes.
  • the resulting mixture containing 2.14% of water was granulated and the granules were dried as in Example 1. Free-flowing granules having a moisture content of 0.05% and an apparent density of 0.49 g/ml were obtained.
  • Example 1 was repeated with the exception that 4 kg of dry sugar powder consisting of 98.5% of fructose and 1.5% of glucose (moisture content 0.15%) and 0.92g of an 88.7% solution of enzymatically isomerized glucose (fructose 46.5%, glucose 53.5%) were used. The kneaded mixture containing 4.1 1% of water was granulated and dried in vacuo. Free-flowing granules having a moisture content of 0.15% and an apparent density of 0.54 g/ml were obtained.
  • Example 1 was repeated with the exception that 4 kg of a mixed sugar powder of fructose and glucose (7:3, moisture content 0.21%) and 0.4 kg of the same syrup as used in the Example 4 were mixed. The resulting mixture containing 2.13% of water was pelletized by the same manner as Example 2 and then dried. Freeflowing pellets having a moisture content of 0.21% and an apparent density of 0.54 were obtained.
  • Example 1 was repeated with the exception that 4 kg of a mixture of fructose and glucose (7:3, moisture content 0.21) and 1.20 kg of an 87.6% solution of the same sugar were mixed. The resulting mixture containing 3.03% of water was granulated and dried. Free flowing granules having a moisture content of 0.08% and an apparent density of 0.54 g/ml were obtained.
  • a method for preparing anhydrous, free-flowing solid particles of a sugar selected from the group consisting of glucose, fructose and admixtures thereof which comprises:
  • a method according to claim 1 wherein said sugar solution is a massecuite wherein 3050% of the total sugar is present in the form of crystals.

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Confectionery (AREA)
  • Seasonings (AREA)
  • Saccharide Compounds (AREA)
US475198A 1973-06-04 1974-05-31 Production of free-flowing particles of glucose, fructose or the mixture thereof Expired - Lifetime US3929503A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP48063250A JPS5012245A (da) 1973-06-04 1973-06-04

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US (1) US3929503A (da)
JP (1) JPS5012245A (da)
DE (1) DE2426437A1 (da)
FR (1) FR2231751B3 (da)
GB (1) GB1466293A (da)

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4199374A (en) * 1978-12-22 1980-04-22 Chimicasa Gmbh Process of preparing crystalline fructose from high fructose corn syrup
US4199373A (en) * 1979-04-13 1980-04-22 Chimicasa Gmbh Process for the manufacture of crystalline fructose
US4237764A (en) * 1977-06-20 1980-12-09 Nippon Gakki Seizo Kabushiki Kaisha Electronic musical instruments
US4517021A (en) * 1983-10-28 1985-05-14 A. E. Staley Manufacturing Company Semi-crystalline fructose
US4640717A (en) * 1984-03-15 1987-02-03 Tate & Lyle Public Limited Company Sugar process
US4676991A (en) * 1986-04-23 1987-06-30 A. E. Staley Manufacturing Company Sweetener composition
US4737368A (en) * 1986-04-23 1988-04-12 A. E. Staley Manufacturing Sweetener composition
US4869907A (en) * 1984-04-18 1989-09-26 Toyo Jozo Kabushiki Kaisha Method of enhancing growth and weight gain in swine and block for use therein
US5015297A (en) * 1985-05-15 1991-05-14 Roquette Freres Method and installation for the production of anhydrous crystalline fructose
US5230742A (en) * 1987-02-02 1993-07-27 A. E. Staley Manufacturing Co. Integrated process for producing crystalline fructose and high-fructose, liquid-phase sweetener
US5234503A (en) * 1987-02-02 1993-08-10 A.E. Saley Manufacturing Co. Integrated process for producing crystalline fructose and a high-fructose, liquid-phase sweetener
US5350456A (en) * 1987-02-02 1994-09-27 A. E. Staley Manufacturing Company Integrated process for producing crystalline fructose and a high fructose, liquid-phase sweetener
WO1995034687A1 (en) * 1994-06-10 1995-12-21 Crompton & Knowles Corporation Process for recrystallizing sugar and product thereof
US5656094A (en) * 1987-02-02 1997-08-12 A.E. Staley Manufacturing Company Integrated process for producing crystalline fructose and a high-fructose, liquid phase sweetener
US6123980A (en) * 1997-12-01 2000-09-26 Imperial Sugar Company Preparing granulated sugar blends and products
ITRM20110376A1 (it) * 2011-07-18 2013-01-19 Luigi Pirrone Dolcificante di origine vegetale costituito da glucosio e fruttosio presenti in concentrazioni variabili, provenienti dalla trasformazione di materie prime di origine vegetale e loro derivati, con addizione o meno di componenti commestibili
WO2020028360A1 (en) 2018-07-30 2020-02-06 Cargill, Incorporated Semi-crystalline fructose in solid form and process for manufacturing the same

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5299004A (en) * 1976-02-17 1977-08-19 Nec Corp Automatic voice responding system
US4162926A (en) * 1978-01-11 1979-07-31 W. R. Grace & Co. Method of drying complex sugar solutions
JPS5829652Y2 (ja) * 1982-03-15 1983-06-29 日本電気株式会社 自動音声応答装置

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3513023A (en) * 1966-04-29 1970-05-19 Boehringer Mannheim Gmbh Process for the production of crystalline fructose
US3816175A (en) * 1972-07-03 1974-06-11 Suomen Sokeri Oy Process for formation of crystalline fructose-glucose blends

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3513023A (en) * 1966-04-29 1970-05-19 Boehringer Mannheim Gmbh Process for the production of crystalline fructose
US3816175A (en) * 1972-07-03 1974-06-11 Suomen Sokeri Oy Process for formation of crystalline fructose-glucose blends

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4237764A (en) * 1977-06-20 1980-12-09 Nippon Gakki Seizo Kabushiki Kaisha Electronic musical instruments
US4199374A (en) * 1978-12-22 1980-04-22 Chimicasa Gmbh Process of preparing crystalline fructose from high fructose corn syrup
US4199373A (en) * 1979-04-13 1980-04-22 Chimicasa Gmbh Process for the manufacture of crystalline fructose
US4517021A (en) * 1983-10-28 1985-05-14 A. E. Staley Manufacturing Company Semi-crystalline fructose
US4640717A (en) * 1984-03-15 1987-02-03 Tate & Lyle Public Limited Company Sugar process
US4869907A (en) * 1984-04-18 1989-09-26 Toyo Jozo Kabushiki Kaisha Method of enhancing growth and weight gain in swine and block for use therein
US5015297A (en) * 1985-05-15 1991-05-14 Roquette Freres Method and installation for the production of anhydrous crystalline fructose
US4676991A (en) * 1986-04-23 1987-06-30 A. E. Staley Manufacturing Company Sweetener composition
US4737368A (en) * 1986-04-23 1988-04-12 A. E. Staley Manufacturing Sweetener composition
US5234503A (en) * 1987-02-02 1993-08-10 A.E. Saley Manufacturing Co. Integrated process for producing crystalline fructose and a high-fructose, liquid-phase sweetener
US5230742A (en) * 1987-02-02 1993-07-27 A. E. Staley Manufacturing Co. Integrated process for producing crystalline fructose and high-fructose, liquid-phase sweetener
US5350456A (en) * 1987-02-02 1994-09-27 A. E. Staley Manufacturing Company Integrated process for producing crystalline fructose and a high fructose, liquid-phase sweetener
US5656094A (en) * 1987-02-02 1997-08-12 A.E. Staley Manufacturing Company Integrated process for producing crystalline fructose and a high-fructose, liquid phase sweetener
WO1995034687A1 (en) * 1994-06-10 1995-12-21 Crompton & Knowles Corporation Process for recrystallizing sugar and product thereof
US5549757A (en) * 1994-06-10 1996-08-27 Ingredient Technology Corporation Process for recrystallizing sugar and product thereof
US5779805A (en) * 1994-06-10 1998-07-14 Crompton & Knowles Corporation Process for recrystallizing sugar and product thereof
US6074489A (en) * 1994-06-10 2000-06-13 Chr. Hansen, Inc. Process for recrystallizing sugar and product thereof
US6123980A (en) * 1997-12-01 2000-09-26 Imperial Sugar Company Preparing granulated sugar blends and products
ITRM20110376A1 (it) * 2011-07-18 2013-01-19 Luigi Pirrone Dolcificante di origine vegetale costituito da glucosio e fruttosio presenti in concentrazioni variabili, provenienti dalla trasformazione di materie prime di origine vegetale e loro derivati, con addizione o meno di componenti commestibili
WO2020028360A1 (en) 2018-07-30 2020-02-06 Cargill, Incorporated Semi-crystalline fructose in solid form and process for manufacturing the same
US11814691B2 (en) 2018-07-30 2023-11-14 Cargill, Incorporated Semi-crystalline fructose in solid form and process for manufacturing the same

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Publication number Publication date
GB1466293A (en) 1977-03-02
DE2426437A1 (de) 1974-12-19
AU6933474A (en) 1975-11-27
FR2231751A1 (da) 1974-12-27
JPS5012245A (da) 1975-02-07
FR2231751B3 (da) 1977-04-08

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