WO2007076640A1

WO2007076640A1 - A method for simultaneously preparing 55 % high fructose syrup and 42 % fructose syrup

Info

Publication number: WO2007076640A1
Application number: PCT/CN2006/000012
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: 2007-07-12
Also published as: WO2007076640A8

Abstract

A method for simultaneously preparing high fructose syrup having fructose content of 55% and 42% by weight. The method comprises : using fructose-rich syrup having fructose content of at least 48-52% 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 a high fructose content syrup product in which fructose content is increased to 58-68.6%, then blending the product with said fructose-rich syrup raw material to form high fructose syrup having fructose content of 55%, simultaneously blending the sediment thus obtained with said raw material or said product to form high fructose syrup having fructose content of 42%.

Description

Method for simultaneously preparing 55% high fructose syrup and 42% fructose syrup

The present invention relates to a method for producing a sweetener, and more particularly to a process for producing fructose syrup. Background technique '

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 for preparing high-fructose syrup containing 55% fructose is generally carried out. First, glucose is isomerized by glucose isomerase to produce about 56% fructose syrup containing fructose, which is then concentrated and then passed. The adsorption column was separated to obtain a fructose syrup containing more than 90% of fructose. Subsequently, 90% or more of the fructose syrup containing fructose and the fructose syrup containing 42% of fructose were adjusted to obtain a high fructose syrup containing 55% of fructose. The method is complicated, and the syrup containing high glucose and low fructose produced by the separation of the adsorption column needs to be returned to the isomerization process to regenerate about 56% of fructose syrup containing fructose, thereby greatly increasing the production cost.

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 the method, the fructose syrup having a fructose content of about 55% is prepared, and the syrup mixed with the crystallized crystal and the mother liquid must be diluted with another diluent to separate the crystal from the mother liquid, thereby obtaining the desired 55%. Left and right fructose syrup. Therefore, this method is demanding, has many steps, and does not obtain a fructose syrup intermediate having a fructose content of more than 58%.

In the method disclosed in Chinese Patent Publication No. 1063903A, 42% of fructose containing fructose is used. Syrup is used as raw material. However, the solid content is also required to be higher than 75%, and the amount of seed crystal used for crystallization 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 fructose content.

Therefore, there is a need in the art for more relaxed process conditions, and it is possible to simultaneously prepare 42% fructose syrup and 55% fructose syrup which are currently on the market, and does not produce a syrup containing high glucose fructose syrup which requires re-isomerization. The invention has thus been proposed. Summary of the invention

The present invention provides a method of simultaneously preparing a fructose syrup containing 55% and 42% by weight of fructose, comprising:

Providing fructose syrup raw material, wherein the fructose content is 48%-52% of the total weight of the raw material, and the solid content is 70%-75% of the total weight of the raw material;

Adding at least 0.1% by weight of seed crystals to the fructose syrup raw material;

The seeded material is allowed to stand at 4-21 ° C;

Separating the precipitate precipitated from the standing product to obtain a supernatant;

Dissolving the supernatant and the fructose syrup raw material with a fructose having a sugar content of 55%;

The precipitate was formulated with the supernatant or the starting material to a 42% fructose syrup.

In one embodiment of the invention, the resulting fructose content is greater than 58% by weight of the supernatant. Preferably, the supernatant has a fructose content of 62% to 86.6% by weight of the supernatant.

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 of the fructose syrup raw material, the higher the standing temperature. For example, the solid content is 75% by weight and the standing temperature is 18. C-21. C. The solid content was 70% by weight and the standing temperature was 4. (.

In another embodiment of the invention, the seed crystal is a 40-160 mesh glucose particle. The precipitate (40-160 mesh) precipitated in the process of the present invention can also be used as the seed crystal of the present invention. More preferably, it is a glucose particle of 120-160 mesh or a precipitate precipitated in the process of the invention. The glucose 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 process of the present invention does not require an excessively high solids content in the fructose syrup raw material. The solid content may be less than 75%, and the setting temperature in the crystallization process may be adjusted as the solid content changes, and the applicability is strong. In addition, the supernatant is separated by centrifugation and pressing, which is convenient and easy to produce. The prepared fructose 58%-68% high fructose fructose syrup can be blended to produce 42% fructose syrup and 55% fructose syrup. This process has a high throughput and is suitable for large-scale industrial production. The present invention does not require the use of an expensive adsorption method for the preparation of HFCS-55, and the precipitation of high glucose and fructose after crystallization of fructose is directly used for the preparation of HFCS-42. detailed description

The present invention relates to a method for producing 55% high fructose syrup and 42% fructose syrup by first preparing a fructose syrup having a fructose content of up to 58%-68.6% and a by-product of glucose precipitation containing a small amount of fructose, and then passing The product or by-product is separately prepared from the starting materials, or the product is mixed with by-products to produce the desired 55% high fructose syrup and 42% fructose syrup.

In the method of the present invention, 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 may be added thereto as a seed crystal 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 preferably 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 glucose precipitate is separated by a separation method such as centrifugation or pressing. The supernatant after separation of the glucose precipitate has a fructose content of 58% by weight or more, preferably 62% to 68.6% by weight, based on the supernatant.

In the present invention, the fructose syrup raw material has a solid content of 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 amount of fructose 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. Add seed amount The more the crystals are formed, the faster. The glucose particles or the precipitate formed in the method of the present invention can be used as a seed crystal. The seed crystals used are preferably 40-160 mesh glucose particles or precipitates precipitated by the process of the invention. More preferably, it is a 120-160 mesh particle or the precipitated precipitate.

It is preferred to use crystals for the seed crystals. In a preferred embodiment of the invention, 140 crystals of glucose crystals or crystals precipitated by the method 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 rate, the lower the yield of the supernatant, and the higher the fructose content in the supernatant. The present invention uses higher resting temperatures, such as 18-21. C can still obtain fructose syrup containing a higher concentration of fructose. Such temperature ranges capable of implementing the technical solution 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%; the standing temperature is at 18. C-21. At C, the solids content is controlled at 75%.

The fructose content in the syrup raw material is preferably controlled to be 48% to 52% by weight.

In order to prepare 55% high fructose syrup and/or 42% fructose syrup, according to the content of fructose in the supernatant, the supernatant is mixed with the fructose syrup raw material in a certain ratio to prepare a fructose-containing 55. % fructose syrup. Preferably, the precipitate and the fructose syrup raw material or the supernatant are formulated into a fructose syrup containing 42% fructose according to the content of fructose in the precipitate. The determination of the mixing ratio is well known to those skilled in the art depending on the fructose content to be formulated. Thus, the present invention is capable of simultaneously formulating 55% fructose syrup and 42% fructose syrup without the need for additional materials and products. However, it is also within the practice of the present invention to use other fructose syrups of a fructose content different from the present invention in combination with the products, by-products or materials of the present invention during the formulation process.

Unless otherwise stated, the percentages of "content," or "concentration" as used herein are by weight.

The fructose syrup of "high concentration" or "high content" fructose according to the invention means that the fructose content is at least 55%, preferably at least 58%, more preferably at least 62% by weight of fructose syrup, based on the total weight of the fructose syrup . 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 concentration was measured by an ATAGO SMART-1 autorefractometer, 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 content 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 100 g of the syrup raw material containing the total amount of different solids was cooled to room temperature, 0.1 g of 40-80 mesh glucose particle seed crystals were added. After stirring, cool to 10. C, let stand for 10 days. Then truthfully 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 content of solids 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 supernatant (%) 60.56 65.48 67.53 68.03 Precipitate 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 Precipitate 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. Dian. After stirring, it was cooled to 18 ° C and allowed to stand for 5 days. Centrifugation was carried out as in Example 1. The fructose content in the resulting supernatant and precipitate was determined. The results are shown in Table 4. Table 4

Total syrup raw materials (g) 100 100 100

Seed force input (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 sedimentation (%) 26.60 26.42 24.53 Example 5

The composition of the syrup raw materials is as follows: fructose content 50.3%, glucose content 49.7%, total solid content 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 material (g) 100 100 100 100 Seed crystal addition amount (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 sedimentation (%) 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 particles was added. After stirring, cool to 4-21. C, let stand for 6 days. Centrifugation as described in Example 1 Leaving. The fructose content in the obtained supernatant and precipitate was measured separately. The results are shown in Table 6.

Table 6

Standing temperature (:. C) 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 Example 7

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 resulting supernatant and precipitate was determined 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 Precipitated fructose 17.04 17.38 17.96 20.11 20.63 19.24 18.67 19.06 Content (%) The syrup raw material composition 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 particles was added. After stirring, cool to 4-18. C, let stand for 6 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 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 100 g of the syrup raw material was cooled to room temperature, 0.1 g of 40-80 mesh glucose particles was added. Stir and cool to 10 after stirring. 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 Sediment 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%.

Cool 2,417 grams of syrup to 18. After C, 24.10 g of 40-80 mesh glucose crystals were added. After stirring evenly, it was allowed to stand for 6 days, stirred and mixed, and then sampled 2,240 g, and separated by a press of a Shenzhen Jie kitchen press to obtain 1,368 g of a supernatant and 850 g of a precipitate. The resulting supernatant had a fructose content of 63.73%; the resulting precipitated fructose content was 28.48%. Example 11

The fructose syrup was concentrated to a fructose syrup having a total solid content of 72%, a fructose content of 50.29%, and a glucose content of 49.71% as a raw material.

100 g of the starting material was taken and 0.1 g of 40-80 mesh glucose particles was added. Cool to 12 with a little stirring. C, let stand for 12 days. Centrifugation was carried out as described in Example 1, to give a supernatant of 72.53 g and a precipitate of 27.47 g.

The obtained supernatant had a fructose content of 63.83% and a glucose content of 36.17%.

The resulting precipitate had a fructose content of 19.97% and a glucose content of 80.03%.

72.53 g of the above supernatant was mixed with 129.40 g of the above fructose syrup raw material to obtain a high content of fructose syrup of 201.93 g. The solid content is 70.75%, the fructose content is 55%, and the glucose content is 45%.

27.47 g of the above precipitate was mixed with 82.70 g of the above fructose syrup raw material to obtain 110.17 g of fructose syrup. The total solid content was 74.39%, the fructose content was 42%, and the glucose content was 58%. Example 12

The fructose syrup was concentrated to a fructose syrup having a total solid content of 75%, a fructose content of 50.13%, and a glucose content of 49.87% as a raw material.

Take 100 grams of raw material and add 1 gram of about 100 mesh water glucose particles. After stirring 18 . C is allowed to stand for 6 days. Centrifugation was carried out as described in Example 1, to obtain a supernatant of 75.79 g and a precipitate of 24.21 g.

The obtained supernatant had a fructose content of 60.33% and a glucose content of 39.67%.

The resulting precipitate had a fructose content of 17.92% and a glucose content of 82.08%.

75.79 grams of the above supernatant and 79.28 grams of the above fructose syrup raw materials are mixed and blended to obtain 155.07 g of fructose syrup with high concentration of fructose. The total solid content was 73.88%, the fructose content was 55%, and the glucose content was 45%.

24.21 g of the above precipitate was mixed with 80.97 g of the above fructose syrup raw material to obtain 105.18 g of fructose syrup. The total solid content was 76.97%, the fructose content was 42%, and the glucose content was 58%. Example 13

100 g of the starting material was taken, and 1 g of the precipitate obtained in Example 1 was added, and after stirring, it was cooled to 18. C, let stand for 5 days. Centrifugation was carried out as described in Example 1, to obtain a supernatant of 73.40 g and a precipitate of 26.60 g.

The obtained supernatant had a fructose content of 60.23% and a glucose content of 39.77%.

The resulting precipitate had a fructose content of 26.42% and a glucose content of 73.58%.

73.40 g of the above supernatant was mixed with 76.31 g of the above raw materials to obtain 149.71 g of high-fruit candy syrup. The total solid content was 73.83%, the fructose content was 55%, and the glucose content was 45%.

26.60 g of the above precipitate was mixed with 55.92 g of the above starting materials to obtain 82.52 g of fructose syrup, the total solid content was 77.35%, the fructose content was 42%, and the glucose content was 58%.

It is to be understood that the embodiments and the embodiments of the present invention are described by way of example only, and those skilled in the art Various modifications and changes are intended to be included within the scope of the appended claims.

Claims

Claim

A method of simultaneously preparing fructose syrup containing 55% and 42% by weight of fructose, comprising:

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;

The precipitate was mixed with the supernatant or the raw material to prepare a fructose syrup having a sugar content of 42%.

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

The method according to claim 1 or 1, wherein the supernatant has a fructose content of 62% to 68.6% by weight of the supernatant.

The method according to any one of claims 1 to 3, wherein the standing temperature is 18 ° C to 21 ° C.

5. The method of claim 4, wherein the solids content is 75% of the total weight of the feedstock.

The method according to any one of claims 1 to 3, wherein the solid content is 70% of the total weight of the raw material, and the standing temperature is 4. C.

The method according to any one of claims 1 to 6, wherein the seed crystal is from 1% to 5% by weight based on the total weight of the raw material.

The method according to any one of claims 1 to 7, wherein the seed crystal is a 40-160 mesh glucose particle or the precipitated precipitate.

9. The method of claim 8, wherein the seed crystal is a 120-160 mesh glucose particle or the precipitated precipitate. '

10. The method of claim 8 or 9, wherein the glucose particles or the precipitated precipitate are crystalline.

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