WO2007079606A1

WO2007079606A1 - A method for preparing high concentration fructose-containing high fructose syrup by crystallization

Info

Publication number: WO2007079606A1
Application number: PCT/CN2006/000013
Authority: WO
Inventors: Jun Wang; Junming Chen
Original assignee: Bioright Worldwide Company Ltd.
Priority date: 2006-01-06
Filing date: 2006-01-06
Publication date: 2007-07-19

Abstract

A method for preparing high concentration fructose-containing high fructose syrup. The method comprises: using fructose-rich syrup having fructose content of more than 42% and solid content of 70-75% by weight as the raw material, adding crystal seeds and cooling to crystallize, separating the sediment by centrifuging or squeezing, thereby obtaining high fructose syrup having high concentration fructose in which fructose content is increased to 58-68.6%. The method of the invention is simple and easy to operation, has high yield, can obtain high fructose content, and doesn't need fructose-rich syrup having too high fructose content as the raw material.

Description

Preparation of fructose syrup with high concentration of fructose by crystallization method

The present invention relates to a novel process for preparing fructose syrup containing more than 58% by weight of fructose. technical background

Fructose syrup is a new type of sweetener that was put into industrial production in the 1970s. It is suitable for a variety of foods. Its sugar composition is mainly fructose and glucose. According to ISBI (International Association of Beverage Science and Technology) international standards, there are two main types of fructose syrup that have been commercialized in the international market. One is fructose syrup or HFCS-42 with a fructose content of 42%; the other is fructose. It is 55% fructose syrup, which is called high fructose syrup or HFCS-55.

Nowadays, the production process of industrially preparing high fructose syrup with 55% fructose content generally firstly isomerizes glucose to glucose isomerase to produce about 56% fructose syrup containing fructose, which is then concentrated and then adsorbed. The column was separated to obtain a fructose syrup containing more than 90% of fructose. Subsequently, fructose syrup containing more than 90% of fructose and fructose syrup containing 42% of fructose were adjusted to obtain a high fructose syrup containing 55% of fructose.

In addition to the use of adsorption columns, fructose can also be enriched by crystallization by virtue of its high solubility in aqueous solution over glucose.

U.S. Patent No. 4,634,472 discloses the preparation of high fructose syrup containing high concentrations of fructose by crystallization, but requires that the solids content of the fructose syrup raw material must be above 75%. If it is less than 75%, no crystals are formed, so that fructose syrup having a high concentration of fructose cannot be produced. It is also required that the seed crystal used for crystallization has a particle size of 200 mesh. In this method, it is also necessary to dilute the syrup mixed with the crystals and the mother liquid to separate the crystals from the mother liquid, thereby obtaining a fructose syrup containing a high concentration of fructose. The fructose syrup obtained has a fructose content of about 55%, and generally does not exceed 58%. Therefore, this method is demanding, has many steps, and the fructose content obtained is relatively low.

In the method disclosed in Chinese Patent Publication No. 1063903A, fructose syrup containing 42% fructose is used as a raw material. The solids content of the raw materials in the examples thereof were all higher than 75%. And used for The amount of crystal seeds used is large, generally 5-30%. In the syrup after crystallization, the fructose content generally does not exceed 58%. Therefore, the method also has the defect that the condition requires strict product with low fructose content.

Therefore, there is a need in the art for a process for preparing a fructose syrup which is more lenient in process conditions, has a good process, and has a high yield but a higher fructose content in the product. Summary of the invention

The present invention relates to a method for preparing a fructose syrup containing a high concentration of fructose, comprising: providing a fructose syrup raw material, wherein the fructose content is more than 42% by weight of the total weight of the raw material, and the solid content is the total weight of the raw material. 70-75%;

Adding at least 0.1% of seed crystals to the fructose loading material; - allowing the seeded material to stand at a temperature of 4-21 ° C;

The precipitate precipitated in the standing product is separated, and the obtained supernatant is a fructose syrup containing a high concentration of fructose.

The fructose syrup obtained by the process of the invention has a fructose content of greater than 58% by weight.

In one embodiment of the invention, the resulting supernatant has a fructose content of from 58% to 68.6% by weight of the supernatant. Preferably, the supernatant has a fructose content of 62%-68.6% by weight of the supernatant.

In a preferred embodiment of the invention, the fructose content of the feedstock may range from 48 to 52% by weight.

In a particularly preferred embodiment of the invention, the standing temperature is 18. C -21 ⁰ C.

In an embodiment of the invention, the higher the solids content, the higher the standing temperature. For example, the solid content is 75% by weight, the standing temperature may be 18 ° C - 21 ° C; and when the solid content is 70 % by weight, the standing temperature may be 4. C.

In another embodiment of the invention, the seed crystals used are 40-160 mesh glucose particles. The precipitate (40-160 mesh) precipitated in the process of the present invention can also be used as a seed crystal of the present invention. Preferably, the 120-160 mesh glucose particles, and the precipitate precipitated in the process of the present invention are further used as seed crystals of the present invention. The particles or precipitates in crystalline form are most preferred in the present invention.

In the process of the invention, the separation can be carried out by centrifugation or press separation. Those skilled in the art can select according to a specific process. Unlike the prior art, the method of the present invention does not require an excessively high solids content in the fructose syrup raw material. The solids content may be less than 75%, and the standing temperature during crystallization may be adjusted accordingly depending on the solid content. In addition, the supernatant is separated by centrifugation or pressing, and the operation is simple. Therefore, the method of the present invention can also obtain a fructose syrup having a high yield and a high fructose concentration of 58% to 68% at a solid content of less than 75%, and is suitable for large-scale industrial production. detailed description

As described above, the present invention provides a method of preparing fructose syrup containing a high concentration of fructose. In the obtained fructose syrup, the fructose content can be as high as 58% to 68.6% by weight.

In the method of the present invention, fructose having a fructose content of 42% by weight or more is preferably used, and fructose syrup having a fructose content of 48% to 52% and a solid content of 70 to 75% by weight is preferably used as a raw material.

The process of the invention can be carried out in a conventional container. For example, the raw material is placed in a crystallizing tank, and 0.1% or more of glucose particles or a precipitate produced by the present invention is added as a seed crystal to the crystallizing tank at room temperature. The syrup in the crystallization vessel is then at 4-21. Stir under C and let stand. It is preferably allowed to stand for 5-12 days. It is particularly preferred at 18. C-21. Let stand at the temperature of C. A glucose precipitate containing a small amount of fructose was precipitated. Finally, the precipitated precipitate is separated by a separation method such as centrifugation or pressing. The supernatant after separation and precipitation has a fructose content of 58% by weight or more, preferably 62% to 68.6% by weight, based on the supernatant.

In the method of the present invention, the solid content of the fructose syrup raw material is from 70% to 75% by weight. The higher the solid content, the greater the amount of crystals formed, the lower the amount of supernatant, and the higher the fructose content in the supernatant.

In the present invention, the amount of the seed crystal may range from 0.1% to 5% by weight of the raw material. The more seed crystals are added, the faster the rate of crystal formation. Small glucose particles, or precipitates formed in the method of the invention, may be used as seed crystals. The seed crystal used is preferably a 40-160 mesh glucose particle or a precipitate precipitated by the method of the present invention, more preferably a 120-160 mesh particle.

It is preferred to use crystals for the seed crystals. In a preferred embodiment of the invention, about 180 mesh glucose crystals or crystals precipitated in the process of the invention are used as seed crystals in an amount of from 1% to 2% by weight based on the total amount of the syrup material. The standing temperature is usually maintained at 4-21. C, to facilitate crystallization of the seed crystal-containing syrup. The lower the temperature, the greater the amount of crystals formed, the faster the crystallization rate, the lower the yield of the supernatant, and the higher the fructose content in the supernatant. The resting temperature of the present invention is different from the resting temperature of the prior art, and the present invention uses a higher resting temperature, for example, 18-21. C can still obtain fructose syrup containing a higher concentration of fructose. Such temperature ranges capable of implementing the technical solutions of the present invention are not disclosed in the prior art.

Considering the above factors, when the standing temperature is low, the total solid content of the syrup raw material used may be slightly lower; when the standing temperature is high, the total solid content of the syrup raw material used should be correspondingly increased. For example, the standing temperature is 4. When C is around, the solid content should be controlled at about 70%; when the temperature is between 18 °C and 21 °C, the solid content is controlled at 75%.

The percentages of "content" or "concentration" as used herein are by weight unless otherwise indicated.

The fructose syrup of the "high concentration" or "high content" fructose of the present invention refers to a fructose syrup having a fructose content of at least 55%, preferably at least 58%, more preferably at least 62% by weight based on the total weight of the syrup.

The method of the present invention does not require an excessively high solids content in the fructose syrup raw material. For example, it is not required to be more than 75%, and the crystal standing temperature can be adjusted as the solid content changes. A high yield of fructose syrup containing a high concentration of fructose can also be obtained at less than 75%. Moreover, higher fructose syrups higher than 58% can be obtained in high yield.

The invention is illustrated by the following non-limiting examples. Example

The fructose syrup raw materials in the following examples were prepared from crystalline glucose and crystalline fructose at the concentrations described below unless otherwise stated. The solid content was measured by an ATAGO SMART-1 automatic refractometer, and the fructose content was measured by an automatic polarimeter (wzz-2s digital automatic polarimeter, Shanghai Precision Scientific Instrument Co., Ltd.). The total amount of syrup and the supernatant yield were determined by weighing; sediment weight = total syrup - supernatant production. Example 1

The composition of the syrup raw materials is as follows: fructose content 50.29%, glucose content 49.71%, solid form The content is 70%-75%.

After 100 g of the syrup raw material containing the total amount of different solids was cooled to room temperature, 0.1 g of a 40-80 mesh glucose particle seed crystal was added. Stir and cool to 12 after stirring. C, let stand for 12 days. Centrifugal separation (31,000 g, 15 minutes). The content of fructose in the obtained supernatant and precipitate was measured. The results are shown in Table 1.

Table 1

Total solid content of raw materials (%) 70 72 74 74.9

Total syrup raw materials (g) 100 100 100 100

Supernatant production (g) 84.03 72.53 65.50 62.73

Fructose content in the supernatant (%) 56.65 63.83 66.61 67.34

Precipitation weight (g) 15.97 27.47 34.50 38.27

Fructose content in sedimentation (%) 20.14 19.97 22.44 24.78 Example 2

The composition of the syrup raw materials is as follows: fructose content 50.29%, glucose content 49.71%, total solid content 70%-75%.

After cooling 100 g of the syrup raw material containing the total amount of different solids to room temperature, 0.1 g of 40-80 mesh glucose granule seeds were added. Stir and cool to 10 after stirring. C, let stand for 10 days. Then, centrifugation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 2. Table 2

Total solids content in raw materials (%) 70 72 74 74.9 Total syrup raw materials (g) 100 100 100 100

Supernatant yield (g) 78.05 70.15 63.75 60.05 Fructose content in the supernatant (%) 60.56 65.48 67.53 68.03 Precipitation weight (g) 21.95 29.85 36.25 39.95 Fructose content in sedimentation (%) 20.84 22.36 25.60 25.73 Example 3 The composition of the syrup raw materials is as follows: fructose content 50.32%, glucose content 49.71%, total solid content 72%-75%.

After 100 g of the syrup raw material was cooled to room temperature, 1 g of the precipitate precipitated in Example 1 was added. Stir and cool to 18 after stirring. C, let stand for 5 days. Centrifugation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 3. table 3

Total solids in raw materials (%) 72 73 74 75

Total syrup raw materials (g) 100 100 100 100

Supernatant yield (g) 85.47 81.07 75.80 73.40 Fructose content in supernatant (%) 55.67 57.43 58.97 60.23 Precipitation weight (g) 14.53 18.93 24.20 26.60 Fructose content in sedimentation (%) 22.92 24.35 25.61 26.42 Example 4

The composition of the syrup raw materials is as follows: fructose content 50.32%, glucose content 49.71%, total solid content 75%.

After 100 g of this syrup raw material was cooled to room temperature, 0.5-2 g of the precipitate precipitated in Example 1 was added. Stir and cool to 18 after stirring. C, let stand for 5 days. Centrifugation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 4. Table 4

Total syrup raw materials (g) 100 100 100

Seed crystal addition amount (g) 0.5 1.0 2.0

Supernatant production (g) 75.40 73.40 73.60

Fructose content in the supernatant (%) 59.10 60.23 61.03

Sediment weight (g) 3.59 3.92 3.89

Fructose content in precipitation (%) 26.60 26.42 24.53 Example 5 The composition of the syrup raw materials is as follows: fructose content is 50.3%, glucose content is 49.7%, and total solid content is 72%.

After 100 g of this syrup raw material was cooled to room temperature, 0.1-5 g of 40-80 mesh crystalline glucose granules were added. Stir and cool to 15. C, let stand for 7 days. Centrifugal separation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 5. table 5

Total syrup raw materials (g) 100 100 100 100 Seeds (g) 0.1 0.5 1.0 5.0 Supernatant yield (g) 88.60 84.35 81.80 74.65 Fructose content in supernatant (%) 54.46 56.67 57.84 59.59 Sediment weight (g 11.4 15.65 18.20 25.35 Fructose content in precipitation (%) 22.23 18.66 18.42 16.82 Example 6

The composition of the syrup raw materials is as follows: the total solid content is 75.00%, the fructose content is 50.13%, and the glucose content is 49.87%.

After cooling 100 g of the syrup raw material to room temperature, 1 g of 120-160 mesh monohydrate glucose granules was added. After stirring, cool to 4-2] ° C and let stand for 6 days. Centrifugal separation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 6. Table 6

Standing temperature (.€) 4 18 21

Total syrup raw materials (g) 100 100 100

Supernatant production (g) 59.30 75.79 78.60

Fructose content in the supernatant (%) 65.58 60.33 58.32

Precipitation weight (g) 41.7 26.35 25.96

Fructose content in sedimentation (%) 21.56 17.92 21.56 The composition of the syrup raw materials is as follows: the total solid content is 72.00-75.00%, the fructose content is 50.30%, and the glucose content is 49.70%.

After 100 g of this syrup material was cooled to room temperature, 0.3 g of 40-80 mesh glucose particles were added. Stir and cool to 15-18. C, let stand for 12 days. Centrifugation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 7. Table 7

Standing temperature 15 15 15 15 18 18 18 18

(°C)

Solids in raw materials 72 73 74 75 72 73 74 75 Concentration (%)

Total syrup raw materials 100 100 100 100 100 100 100 100 quantity (g)

Supernatant yield (g) 82.45 82.20 75.20 71.80 87.45 81.55 79.50 76.25 Fructose in the supernatant 58.30 61.17 62.74 63.17 55.04 58.03 59.86 60.96 Content (%:)

Precipitation weight (g) 17.55 17.80 24.80 28.20 12.55 18.45 20.50 23.75 Fructose in precipitation 17.04 17.38 17.96 20.11 20.63 19.24 18.67 19.06 Content (%) Example 8

The composition of the syrup raw materials is as follows: The total solid content is 72.00-75.00%, and the fructose content is 48-52%. After cooling 100 g of the syrup raw material to room temperature, 1 g of 120-160 mesh monohydrate glucose granules was added. After stirring, it was cooled to 4-18 ° C and allowed to stand for 6 days. Centrifugal separation was carried out as described in Example 1. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 8.

Table 8 Standing temperature (°c) 4 4 4 18 18 18 Fructose content in raw materials (%) 48 50 52 48 50 52 Solids concentration in raw materials (%) 70 70 70 75 75 75 Total syrup raw materials (g) 100 100 100 100 100 100 Supernatant yield (g) 76.70 79.88 83.84 70.94 75.79 81.44 Fructose content (%) 60.36 60.74 60.63 61.30 60.33 59.19 Sediment weight (g) 23.30 20.12 16.16 29.06 24.21 18.56 Fructose content in sediment (%) 16.79 17.92 19.08 16.79 17.92 19.08 Example 9

The composition of the syrup raw materials is as follows: The total content of solids is 72%-74.9%, and the fructose content is 50.29%.

After cooling 100 g of the syrup raw material to room temperature, 0.1 g of 40-80 mesh glucose granules was added, and after stirring, it was cooled to 10. C. Allow to stand for 14 days. After wrapping with an industrial polyester cloth 260, the supernatant is squeezed by hand. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 9. Table 9

Solids concentration in raw materials (%) 70 72 74 74.9

Total syrup raw materials (g) 100 100 100 100

Supernatant yield (g) 75.93 70.93 66.13 60.50 Fructose content (%) 63.26 65.74 67.38 68.60 Precipitation weight (g) 24.07 29.07 34.87 39.50 Fructose content in sedimentation (%) 20.06 21.64 24.22 27.78 Example 10

The composition of the syrup raw materials is as follows: The total solid content is 75.01%, and the fructose content is 50.26%.

2,417 grams of syrup was cooled to 18. After C, 24.10 grams of 40-80 mesh glucose crystals were added. After stirring evenly, it was allowed to stand for 6 days. After mixing and mixing, 2,240 g was sampled and separated by a press of Shenzhen Jie Kitchen Company. The supernatant was 1,368 g and the precipitate was 850 g. The obtained supernatant had a fructose content of 63.73%; the obtained precipitated fructose content was 28.48%. It is to be understood that the embodiments and the embodiments of the present invention are intended to be illustrative only, and that those skilled in the art, in light of the scope of the invention, Such modifications and variations are intended to be included within the scope of the appended claims.

Claims

Claim

A method of preparing fructose syrup of high concentration fructose, comprising:

Providing fructose syrup raw material, wherein the fructose content is more than 42% of the total weight of the raw material, and the solid content is 70-75% of the total weight of the raw material;

At least 0.1% by weight of seed crystals are added to the fructose syrup raw material; the seed material after the seeding is added at 4-21. Let stand under C;

2. The method of claim 1 wherein the supernatant has a fructose content of greater than 58% of the total weight of the supernatant.

The method according to claim 1 or 2, wherein the supernatant has a fructose content of 62% to 86.6% by weight based on the total weight of the supernatant.

The method according to any one of claims 1 to 3, wherein the fructose raw material has a fructose content of 48 ° / of the total weight of the raw material. -52%.

The method according to any one of claims 1 to 4, wherein the standing temperature is 18 ° C - 21. (:.

6. The method of any of claims 5, wherein the solids content is 75% of the total weight of the feedstock.

The method according to any one of claims 1 to 4, wherein the solid content is 70% of the total weight of the raw material, and the standing temperature is 4. (.

8. The method of any of claims 1-7, wherein the seed crystals comprise from 1% to 5% by total weight of the feedstock.

9. The method of claim 8, wherein the seed crystal is a 40-160 mesh glucose particle or the precipitated precipitate.

10. The method of claim 9, wherein the seed crystal is a 120-160 mesh glucose particle or the precipitated precipitate.

11. A method according to any one of claims 1 to 10 wherein the separation is centrifugation or pressing.