AU2007202885B2

AU2007202885B2 - Process and plant for producing sugar products from grapes

Info

Publication number: AU2007202885B2
Application number: AU2007202885A
Authority: AU
Inventors: Fabio Foraci
Original assignee: NATURALIA INGREDIENTS Srl
Current assignee: NATURALIA INGREDIENTS Srl
Priority date: 2007-06-21
Filing date: 2007-06-21
Publication date: 2014-01-16
Anticipated expiration: 2027-06-21
Also published as: AU2007202885A8; AU2007202885A1

Abstract

PROCESS AND PLANT FOR PRODUCING SUGAR PRODUCTS FROM GRAPES 5 The process for producing sugar products from grapes consists of treating a solution of liquid rectified concentrated must by chromatography, to separate at least one sugar contained in it. The plant for producing sugar products from grapes comprises a plurality of columns 10 connected together in series, each column implementing in succession all the steps of the chromatographic process, but implementing steps of the process which are different from the other columns. A recirculation step is provided in passing from one step to the next. N:\Melbourne\Caeea\Patent\72300-72999\P72322.AU\Specis\P72322.AU GH SPEC.doc 21/06/07

Description

AUSTRALIA Patents Act 1990 COMPLETE SPECIFICATION Standard Patent Applicant(s) CANTINE FORACI S.r.l. Invention Title: Process and plant for producing sugar products from grapes The following statement is a full description of this invention, including the best method for performing it known to me/us: -2 PROCESS AND PLANT FOR PRODUCING SUGAR PRODUCTS FROM GRAPES Technical Field The present invention relates to a process and plant 5 for producing sugar products from grapes. Background Grapes internally contain sugars, in particular glucose and fructose. An aqueous mixture can be extracted from grapes, the 10 aqueous mixture formed from water, fructose and glucose, and known as rectified concentrated must. This mixture can be processed to form rectified concentrated must in crystalline or powder form. In particular, Italian patent application RM99A000662 15 describes a process in which the liquid rectified concentrated must is initially concentrated to a concentration of 820 brix and then mixed with neutral 96* ethyl alcohol, in the proportion of 1:1 (i.e. 50% ethyl alcohol and 50% liquid rectified concentrated must). 20 The mixture of ethyl alcohol and liquid rectified concentrated must is stirred to enable the ethyl alcohol to extract the water contained within the sugars. This operation results in separation into a lower layer of pasty grape sugar and an upper layer of ethyl 25 alcohol and water. 4935582_1 (GHMatters) P72322.AU -3 The mixture of water and ethyl alcohol is then removed and distilled (to recover the ethyl alcohol) while the pasty matter is kept for at least 15 days at a temperature of -5/6 0 C for crystal formation. 5 After the time required for crystal formation (at least 15 days) the crystals are centrifuged, washed and maintained in a dryer to obtain the final product. The final product obtained does not present a true crystalline or powder structure, but instead is in the form of a 10 gelatinous mass, consisting of: glucose and fructose sugars (and other minimal quantities of substances present in the grape defined as "non-sugar"), ethyl alcohol and water. In this respect, the ethyl alcohol removes only part 15 of the water, the final drying not being able to eliminate the remainder of the water, which therefore remains incorporated in the interior of the gelatinous mass without being able to emerge from it. The gelatinous mass is also unstable in air and 20 difficult to work. Another drawback is the high cost of the ethyl alcohol, both at the purchase stage and in its recovery; this evidently affects the cost of the final product. The crystal maturing time is very lengthy and usually 25 varies considerably depending on the particular conditions 4935582_1 (GHMatters) P72322.AU -4 under which it takes place, this leading to difficult industrialization of the process. In addition, crystal washing inevitably modifies the fructose/glucose weight ratio because of the greater water 5 solubility of fructose compared with glucose. To rebalance this ratio an attempt has been made to enrich the starting solution concentrated to 820 brix with the fructose recovered from the wash water and reconcentrated. 10 However the finished product obtained is unsatisfactory in terms of its dryness, taste and smell. The technical aim of the present invention is, therefore, to provide an alternative process for producing sugar products from grapes. 15 The technical aim, together with these and further advantages, are attained, according to the invention, by a process for producing sugar products from grapes in accordance with the accompanying claims. Summary 20 In one embodiment of the invention there is provided a process for producing sugar products from grapes by treating a solution of liquid rectified concentrated must by chromatography, to separate at least one sugar contained in it; wherein it is used in a plant comprising 25 a plurality of columns connected together in series, each column implementing in succession all the steps of the 4935582.1 (GHMatters) P72322.AU -5 chromatographic process, but implementing steps of the process which are different from the other columns, a recirculation step being provided in passing from one step to the next; and at least one of the obtained sugars is 5 separated from the liquid solution containing it. The liquid rectified concentrated must used for separating the sugars may have a concentration of 650 brix. The separated sugars may comprise a liquid solution of glucose and a liquid solution of fructose. 10 The separation may be carried out by crystallization within a metastable region of the treated liquid solution. The crystallization of the fructose may comprise the steps of concentrating the liquid solution of fructose, cooling, fructose crystal growth, and crystal separation from the 15 liquid solution. The process may further comprise a step of seeding with fructose crystals between the concentration step and the cooling step. Within the concentration step, the liquid solution may be brought to a concentration of 80-840 brix. 20 Seeding may be carried out by adding fructose crystals to the liquid solution in a quantity of 0.95-5 wt%. Seeding may also be carried out by adding to the liquid solution fructose crystals of less than 0.15 millimetre in size. 25 The cooling step may be carried out by cooling the liquid solution to a temperature of 10-15 0 C. The cooling 4935582_1 (GHMatters) P72322.AU -6 step may be carried out to a temperature of 10-15*C and preferably to 11-13 0 C. The separation step may be of a centrifugal type. The glucose separation may comprise the steps of 5 concentrating the liquid solution of glucose, cooling and granulating the glucose, and drying the glucose. Within the concentration step, the liquid solution of glucose may be brought to a concentration of 68-82* brix, and preferably to a concentration of 70-74* brix. 10 Granulation may be simultaneous with cooling. The mixture may be stirred during cooling and granulation. The drying step of the process may take place under vacuum. The process may further comprise the mixing together 15 of the glucose separated from its liquid mixture and the fructose separated from its liquid mixture. Within the scope of this technical aim, a further advantage of the invention is to provide a process and plant which enable a crystalline or powder product to be 20 obtained rather than a gelatinous mass. In particular, the process of the present invention enables the water to be removed from the gelatinous mass very efficiently. Another advantage of the invention is to provide a 25 process and plant enabling a finished product to be obtained which is stable in air and easily worked. 4935582_1 (GHMatters) P72322.AU -7 A further advantage of the invention is to provide a process and plant which do not require the use of ethyl alcohol, in this manner enabling the costs associated therewith to be substantially reduced. 5 Another advantage of the invention is to provide a process and plant which can be easily industrialized. A further advantage of the invention is to provide a process and plant enabling a finished product to be obtained which presents satisfactory characteristics in 10 terms of dryness, taste and smell. Further characteristics and advantages of the invention will be more apparent from the description of a preferred but non-exclusive embodiment of the process and plant for producing sugar products from grapes according 15 to the invention, illustrated by way of non-limiting example in the accompanying drawings, in which: Figures 1-4 show the plant of the invention in four different stages of operation. Said figures show a plant for producing sugar 20 products from grape, indicated overall by the reference numeral 1. The plant 1 comprises a plurality of columns 2, 3, 4, 5, connected together in series, each of the columns 2, 3, 4, 5 implementing in succession all the steps of the 25 chromatographic process, but implementing steps of the 4935582_1 (GHMatters) P72322AU -8 process which are different from the other columns 2, 3, 4, 5. Hence in practice, when one of the columns (for example the column 2) is in a predetermined stage of the 5 chromatographic process, column 3 is in a different stage, column 4 in a still different stage, and column 4 in a further stage different from all the preceding stages. Each column opportunely effects all the steps of the chromatographic process, a recirculation step being 10 provided for passing from one step to the next. Specifically, as shown in the figures, the plant comprises four columns which implement a glucose concentration step, a glucose stripping step, a fructose enrichment step and a fructose concentration step. 15 In addition to the columns, the plant is provided with connection lines, a concentration must tank 6, a make-up water feeder 7 and a water heater 8 for heating the water to a predetermined temperature for the process. The plant is also provided with a glucose 20 accumulation tank 10 and a fructose accumulation tank 11. The plant operation is evident from that described and illustrated, and is substantially the following. In Figure 1, column 2 is shown in the absorption stage (for concentrating the glucose) and is fed with a 25 fraction rich in glucose and fructose originating from column 5 (as indicated by the dashed line). 4935582_1 (GHMatters) P72322.AU -9 A glucose-rich fraction is withdrawn from the bottom of column 2 and is fed to the glucose tank 10 (dashed and dotted line). Column 3 is in the purification stage (to implement 5 glucose stripping), and is at rest, without feed or discharge. Column 4 is in the desorption stage (i.e. fructose enrichment), and is fed with water (full line), which is used to displace the glucose fraction contained in it 10 (column 4). The fructose fraction is withdrawn from the bottom of column 4 and is fed to the tank 11 (dashed and double dotted line); however not all the fructose is withdrawn, hence part of the fructose is fed to the next column 5 15 (circled line). Column 5 is in the concentration stage (the fructose is concentrated therein), in which it (column 5) is fed with the residual fraction of column 4 still rich in fructose (circled line), its bottoms, together with fresh 20 must, being fed to column 1 (dashed line). This configuration is maintained by the plant for 6 minutes and 30 seconds (six and a half minutes). After a recirculation step of 19 minutes, the plant then assumes the configuration of Figure 2. 25 In this configuration, column 2 is in the concentration stage, it (column 2) being fed with the 4935582_1 (GHMatters) P72322.AU -10 residual fraction from column 5 still rich in fructose (circled line), the bottoms from this column, together with fresh must, being fed to column 3 (dashed line). Column 3 is in the absorption stage, in which it is 5 fed with the fraction rich in glucose and fructose originating from column 2 and with concentrated must (dashed line); a glucose-rich fraction is withdrawn from the bottom of column 3 and fed to the tank (dashed and dotted line). 10 Column 4 is in the purification stage and is a rest, without feed or discharge. Column 5 is in the desorption stage, and is fed with water (to displace the fructose fraction contained in it, full line), the fructose fraction being withdrawn from its 15 bottom and fed to the tank 11 (dashed and double dotted line), the unextracted fructose being fed to column 2 (circled line). This configuration is maintained by the plant for 6 minutes and 30 seconds (six and a half minutes). 20 After a recirculation step of 19 minutes, the plant then assumes the configuration of Figure 3,. Column 2 is in the desorption stage, and is fed with water (to displace the fructose fraction contained in it, full line), the fructose fraction being withdrawn from its 25 bottom and fed to the tank 11 (dashed and double dotted 4935582_1 (GHMatters) P72322AU -11 line), the unextracted fructose being fed to column 3 (circled line). Column 3 is in the concentration stage, in which it (column 3) is fed with the residual fraction of column 2 5 still rich in fructose (circled line), its bottoms, together with fresh must, being fed to column 4 (dashed line). Column 4 is in the absorption stage, in which it is fed with the fraction rich in glucose and fructose 10 originating from column 3 and with concentrated must (dashed line); a glucose-rich fraction is withdrawn from the bottom of column 4 and fed to the tank (dashed and dotted line). Column 5 is in the purification stage and is a rest, 15 without feed or discharge. This configuration is maintained by the plant for 6 minutes and 30 seconds (six and a half minutes). After a recirculation step of 19 minutes, the plant then assumes the configuration of Figure 4. 20 Column 2 is in the purification stage and is a rest, without feed or discharge. Column 3 is in the desorption stage, and is fed with water (to displace the fructose fraction contained in it, full line), the fructose fraction being withdrawn from its 25 bottom and fed to the tank 11 (dashed and double dotted 4935582_1 (GHMatters) P72322.AU - 12 line), the unextracted fructose being fed to column 4 (circled line). Column 4 is in the concentration stage, in which it is fed with the residual fraction of column 3 still rich 5 in fructose (circled line), the bottoms of column 4, together with fresh must, being fed to column 5 (dashed line). Column 5 is in the absorption stage, in which it is fed with the fraction rich in glucose and fructose 10 originating from column 4 and with concentrated must (dashed line); a glucose-rich fraction is withdrawn from the bottom of column 5 and fed to the tank (dashed and dotted line). This configuration is maintained by the plant for 6 15 minutes and 30 seconds (six and a half minutes). After a further recirculation step of 19 minutes, the plant again assumes the configuration of Figure 1. The described plant implements a process for producing sugar products from grapes. 20 The process consists of treating a solution of liquid rectified concentrated must by chromatography, to separate at least one sugar contained in it. The liquid rectified concentrated must used for separating the sugars has a concentration of 650 brix 25 before treatment, i.e. before being fed to the columns 2 4. 4935582_1 (GHMatters) P72322.AU - 13 The separated sugars comprise a liquid solution of glucose and a liquid solution of fructose. At least one of these obtained sugars is then separated from the liquid solution containing it, this 5 separation being achieved by crystallization in the metastable region of the treated liquid solution (i.e. of the glucose and/or fructose liquid solution). The fructose crystallization comprises the steps of concentrating the liquid solution of fructose, possible 10 seeding with fructose crystals (to limit crystallization time), cooling, fructose crystal growth, and crystal separation from the liquid solution. Advantageously, during the concentration step the liquid solution is brought to a concentration of 80-84* 15 brix. Any subsequent seeding is carried out by adding fructose crystals of less than 0.15 millimetre in size to the liquid solution in a quantity of 0.95-5.00 wt%. Cooling is carried out by cooling the liquid solution 20 to a temperature of 10-15*C, separation being by centrifuge. For example the fructose solution is brought to 820 brix at a temperature of 12'C, and seeding is carried out with 1% of crystals. 25 Drying of the crystals obtained (in a static dryer under vacuum) presented no difficulty, the crystals being 4935582_1 (GHMatters) P72322.AU - 14 stable at ambient temperature under humidity conditions of near or greater than 60%. The glucose separation comprises the steps of concentrating the liquid solution of glucose, cooling and 5 granulating the glucose, and drying the glucose. The concentration of the liquid solution of glucose is brought suitably to 68-82* brix, and preferably to 70 740 brix. Cooling is carried out to a temperature of 10-15 0 C and 10 preferably to 11-13 0 C, granulation being simultaneous with cooling. Advantageously, the mixture is stirred during cooling, granulation and drying under vacuum. For example, the glucose mixture has been 15 concentrated to 720 brix and then brought to a temperature of 12 0 C. The glucose obtained in this manner does not present a crystalline structure, is easily dried in a static dryer and has the form of a powder. 20 Finally, the glucose separated from its liquid mixture and the fructose separated from its liquid mixture are advantageously mixed together to form the rectified concentrated must in crystalline or powder form. It has been found in practice that the process and 25 plant for producing sugar products from grapes according to the invention are particularly advantageous, because 4935582_1 (GHMatters) P72322.AU - 15 they enable rectified concentrated must to be obtained in crystalline or powder form of very high quality. The process and plant for producing sugar products from grapes conceived in this manner are susceptible to 5 numerous modifications and variants , all falling within the scope of the inventive concept; moreover all details can be replaced by technically equivalent elements. In the claims which follow and in the preceding description of the invention, except where the context 10 requires otherwise due to express language or necessary implication, the word "comprise" or variations such as "comprises" or "comprising" is used in an inclusive sense, i.e. to specify the presence of the stated features but not to preclude the presence or addition of further 15 features in various embodiments of the invention. It is to be understood that, if any prior art publication is referred to herein, such reference does not constitute an admission that the publication forms a part of the common general knowledge in the art, in Australia 20 or any other country. 4935582_1 (GHMatters) P72322.AU

Claims

1. A process for producing sugar products from grapes, by treating a solution of liquid rectified concentrated must by chromatography, to separate at least one sugar 5 contained in it, wherein it is used in a plant comprising a plurality of columns connected together in series, each column implementing in succession all the steps of the chromatographic process, but implementing steps of the process which are different from the other columns, a 10 recirculation step being provided in passing from one step to the next; and at least one of the obtained sugars is separated from the liquid solution containing it.

2. A process as clamed in claim 1, wherein the liquid 15 rectified concentrated must used for separating the sugars has a concentration of 650 brix.

3. A process as claimed in claim 1 or claim 2, wherein the separated sugars comprise a liquid solution of glucose 20 and a liquid solution of fructose.

4. A process as claimed in any one of claims 1 to 3, wherein the separation is carried out by crystallization within a metastable region of the treated liquid solution. 25 4935582_1 (GHMatters) P72322.AU - 17

5. A process as claimed in claim 4, wherein crystallization of the fructose comprises the steps of concentrating the liquid solution of fructose, cooling, fructose crystal growth, and crystal separation from the 5 liquid solution.

6. A process as claimed in claim 5, wherein by comprising a step of seeding with fructose crystals between the concentration step and the cooling step. 10

7. A process as claimed in claim 5 or claim 6, wherein in the concentration step, the liquid solution is brought to a concentration of 80-84* brix. 15

8. A process as claimed in claim 6 or claim 7, wherein seeding is carried out by adding fructose crystals to the liquid solution in a quantity of 0.95-5 wt%.

9. A process as claimed in any one of claims 6 to 8 20 wherein seeding is carried out by adding to the liquid solution fructose crystals of less than 0.15 millimetre in size.

10. A process as claimed in any one of claims 5 to 9, 25 wherein cooling is carried out by cooling the liquid solution to a temperature of 10-15 0 C. 4935582_1 (GHMatters) P72322.AU -18

11. A process as claimed in any one of claims 5 to 10, wherein the separation is of centrifugal type. 5

12. A process as claimed in claim 3 or 4, wherein the glucose separation comprises the steps of concentrating the liquid solution of glucose, cooling and granulating the glucose, and drying the glucose. 10

13. A process as claimed in claim 12, wherein in the concentration step, the liquid solution of glucose is brought to a concentration of 68-82* brix, and preferably to a concentration of 70-740 brix. 15

14. A process as claimed in claim 12 or claim 13, wherein cooling is carried out to a temperature of 10-15*C and preferably to 11-13 0 C.

15. A process as claimed in any one of claims 12 to 14, 20 wherein granulation is simultaneous with cooling.

16. A process as claimed in any one of claims 12 to 15 wherein by stirring the mixture during cooling and granulation. 25 4935582_1 (GHMatters) P72322.AU -19

17. A process as claimed in any one of claims 12 to 16, wherein drying takes place under vacuum.

18. A process as claimed in any one of the preceding 5 claims, wherein by mixing together the glucose separated from its liquid mixture and the fructose separated from its liquid mixture.

19. A process for producing sugar products from grapes 10 substantially as hereinbefore described with reference to the accompanying drawings. 4935582_1 (GHMatters) P72322.AU