Method for continuously desalting and decolorizing high fructose corn syrup based on simulated moving bed chromatography

Abstract

The invention discloses a method for continuously desalting and decoloring high fructose corn syrup based on simulated moving bed chromatography, and relates to the technical field of chromatographic separation. The continuous desalting and decolorizing method adopts the simulated moving bed chromatography system formed by connecting the cation simulated moving bed chromatography device and the anion simulated moving bed chromatography device in series to perform continuous desalting and decolorizing on the syrup, and can improve the production efficiency, reduce the personnel investment, greatly improve the utilization rate of resin and reduce the production cost. And the use amount of the regenerant and the deionized water is remarkably reduced due to the mechanical use of the eluent, and the environmental pollution and the subsequent treatment cost are reduced. The continuous desalting and decoloring method is simple and efficient, and can realize efficient desalting and decoloring of syrup on the basis of reducing cost and environmental pollution.

Description

Technical Field

[0001] The present invention relates to the technical field of chromatographic separation, and particularly to a method for continuously desalting and decolorizing fructose-glucose syrup based on simulated moving bed chromatography. Background Art

[0002] Currently, for syrup ion exchange, the cation column and anion column are mostly operated separately. This operation method has low automation, low resin utilization rate, and is prone to leakage problems. The regeneration process consumes a large amount of acid and alkali, leading to environmental pollution problems, and also resulting in relatively high subsequent sewage treatment costs. Summary of the Invention

[0003] The purpose of the present invention is to provide a method for continuously desalting and decolorizing fructose-glucose syrup based on simulated moving bed chromatography to solve the problems existing in the above-mentioned prior art.

[0004] To achieve the above purpose, the present invention provides the following solution:

[0005] The present invention provides a method for continuously desalting and decolorizing syrup based on simulated moving bed chromatography, including the following steps:

[0006] The used simulated moving bed chromatography system is composed of a series-connected cationic simulated moving bed chromatography device and an anionic simulated moving bed chromatography device;

[0007] The cationic simulated moving bed chromatography device is equipped with 20 series-connected chromatographic columns, and the corresponding area of the 20 series-connected chromatographic columns is divided into 3 consecutive series-connected areas: an adsorption area, a regeneration area, and a water washing area; the adsorption area is 12 chromatographic column positions, the regeneration area is 5 chromatographic column positions, and the water washing area is 3 chromatographic column positions;

[0008] The adsorption area, regeneration area, and water washing area of the cationic simulated moving bed chromatography device each have 1 feed inlet and 1 discharge outlet;

[0009] Pump the syrup to be treated into the adsorption area of the cationic simulated moving bed chromatography device. During operation, each area works simultaneously. When the operation time reaches the switching time, each chromatographic column in the cationic simulated moving bed chromatography device moves one column position clockwise, and operates in this way in turn to realize continuous operation of syrup desalting and decolorization;

[0010] The anionic simulated moving bed chromatography device is equipped with 20 series-connected chromatographic columns, and the corresponding area of the 20 series-connected chromatographic columns is divided into 3 consecutive series-connected areas: an adsorption area, a regeneration area, and a water washing area; the adsorption area is 10 chromatographic column positions, the regeneration area is 6 chromatographic column positions, and the water washing area is 4 chromatographic column positions;

[0011] The adsorption zone, regeneration zone, and water washing zone of the anion simulated moving bed chromatography device each have one feed inlet and one discharge outlet;

[0012] The syrup processed by the adsorption zone of the cation simulated moving bed chromatography device is introduced into the adsorption zone of the anion simulated moving bed chromatography device. During operation, each zone works simultaneously. When the running time reaches the switching time, each chromatographic column in the anion simulated moving bed chromatography device moves one column position clockwise. It operates in this way successively to achieve continuous desalination and decolorization of the syrup, and the desalted and decolorized syrup is collected at the discharge outlet of the adsorption zone of the anion simulated moving bed chromatography device.

[0013] Further, in the cation simulated moving bed chromatography device and the anion simulated moving bed chromatography device: The feed inlet of the adsorption zone is the first chromatographic column in the clockwise direction of this zone; The feed inlets of the regeneration zone and the water washing zone are the last chromatographic columns in the clockwise direction of these zones.

[0014] Further, the cation simulated moving bed chromatography device is filled with cation resin; The cation resin is 001×7 or D001FD; The anion simulated moving bed chromatography device is filled with anion resin; The anion resin is D301, D354FD, ZGA355FD, or ZGA352MB.

[0015] Further, the ratio of the total mass of the cation resin in the cation simulated moving bed chromatography device to the total mass of the anion resin in the anion simulated moving bed chromatography device is 1:2.

[0016] Further, the operating temperature of the simulated moving bed chromatography system is 50 - 60°C; The switching time is 1000s - 1500s.

[0017] Further, for the cation simulated moving bed chromatography device: During continuous desalination and decolorization, the chromatographic column in the adsorption zone receives the syrup to be desalted and decolorized, the chromatographic column in the regeneration zone receives 5wt% hydrochloric acid, and the chromatographic column in the water washing zone receives deionized water.

[0018] Further, the flow rate of the syrup to be desalted and decolorized is 3 - 5 BV / h, the flow rate of the 5wt% hydrochloric acid is 5 - 10 BV / h, and the flow rate of the deionized water is 5 - 12 BV / h.

[0019] Further, for the anion simulated moving bed chromatography device: During continuous desalination and decolorization, the chromatographic column in the adsorption zone receives the syrup processed by the adsorption zone of the cation chromatography device, the chromatographic column in the regeneration zone receives 4wt% sodium hydroxide, and the chromatographic column in the water washing zone receives deionized water.

[0020] Further, the flow rate of the treated syrup is 3 - 5 BV / h, the flow rate of the 4 wt% sodium hydroxide is 7 - 12 BV / h, and the flow rate of the deionized water is 8 - 15 BV / h.

[0021] Further, the syrup is fructose syrup; the concentration of the syrup is 10% - 30%, the conductivity is 0 - 1000 μs / cm and not 0 μs / cm; the chromaticity is 0 - 200 RBU and not 0 RBU. After being treated by the present invention, the conductivity of the syrup < 50 μs / cm and the chromaticity < 10 RBU.

[0022] The present invention discloses the following technical effects:

[0023] The continuous desalination and decolorization method of the present invention can improve production efficiency, reduce personnel input, and greatly improve the utilization rate of the resin (increase by about 10% - 20%). In the present invention, the reuse of the eluent significantly reduces the consumption of the regenerant and deionized water (reduce by about 20% - 30%), and reduces environmental pollution and subsequent treatment costs.

[0024] The continuous desalination and decolorization method of the present invention is simple and efficient, and can achieve efficient desalination and decolorization of syrup on the basis of reducing costs and environmental pollution. Detailed Embodiments

[0025] The various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, characteristics, and embodiments of the present invention.

[0026] It should be understood that the terms used in the present invention are only for describing particular embodiments and are not intended to limit the present invention. Additionally, for the numerical ranges in the present invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Any intermediate value within any stated value or stated range, as well as each smaller range between any other stated value or intermediate value within the stated range, is also included in the present invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0027] Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the present invention pertains. Although the present invention only describes preferred methods and materials, any methods and materials similar or equivalent to those described herein can also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials related to the documents. In case of conflict with any incorporated document, the content of this specification shall prevail.

[0028] Without departing from the scope or spirit of the present invention, various modifications and variations can be made to the specific embodiments of the description of the present invention, which are obvious to those skilled in the art. Other embodiments obtained from the description of the present invention are obvious to those skilled in the art. The description and examples of the present invention are merely exemplary.

[0029] Regarding the use of "comprising", "including", "having", "containing", etc. in this article, they are all open-ended terms, meaning including but not limited to.

[0030] The embodiment of the present invention uses fructose syrup after liquefaction, saccharification and activated carbon decolorization of corn starch as the raw material. The syrup concentration is 20%, the conductivity is 450 μs / cm, and the chromaticity is 62 RBU.

[0031] Example 1

[0032] A continuous desalination and decolorization method of fructose syrup based on simulated moving bed chromatography:

[0033] The used simulated moving bed chromatography system is composed of a cationic simulated moving bed chromatography device and an anionic simulated moving bed chromatography device connected in series. The operating temperature of the simulated moving bed chromatography system is 50 °C, and the switching time is 1200 s.

[0034] The cationic simulated moving bed chromatography device is equipped with 20 chromatographic columns connected in series (filled with cation resin 001×7). The area corresponding to the 20 chromatographic columns connected in series is divided into 3 consecutive areas connected in series: adsorption area, regeneration area and water washing area; the adsorption area has 12 chromatographic column positions, the regeneration area has 5 chromatographic column positions, and the water washing area has 3 chromatographic column positions. Each area has 1 feed inlet and 1 discharge outlet. The feed inlet of the adsorption area is the first chromatographic column of this area (in the clockwise direction), and the feed inlets of the regeneration area and the water washing area are the last chromatographic column of this area (in the clockwise direction). The syrup is pumped into the adsorption area of the cationic simulated moving bed chromatography device. During the operation, each area works simultaneously. When the operation time reaches the switching time, each chromatographic column moves one column position clockwise, and continuous operation is achieved in this way. During the continuous desalination and decolorization process, the chromatographic columns in the adsorption area are fed with fructose syrup to be desalted and decolorized (flow rate is 4.5 BV / h), the chromatographic columns in the regeneration area are fed with 5 wt% hydrochloric acid (flow rate is 7 BV / h), and the chromatographic columns in the water washing area are fed with deionized water (flow rate is 10 BV / h).

[0035] The anion simulated moving bed chromatography device is equipped with 20 chromatographic columns connected in series (filled with anion resin D301). The area corresponding to these 20 series-connected chromatographic columns is divided into 3 consecutive series-connected areas: the adsorption area, the regeneration area, and the water washing area. There are 10 chromatographic column positions in the adsorption area, 6 chromatographic column positions in the regeneration area, and 4 chromatographic column positions in the water washing area. Each area has 1 feed inlet and 1 discharge outlet. The feed inlet of the adsorption area is the first chromatographic column in this area (in the clockwise direction), and the feed inlets of the regeneration area and the water washing area are the last chromatographic columns in their respective areas (in the clockwise direction). The syrup processed by the adsorption area of the cation simulated moving bed chromatography device is fed into the adsorption area. During operation, each area works simultaneously. When the running time reaches the switching time, each chromatographic column moves one column position clockwise. Continuous operation is achieved by running in this way successively, and the desalted and decolorized syrup is collected at the discharge outlet of the adsorption area of the anion simulated moving bed chromatography device. During the continuous desalting and decolorization process, the chromatographic columns in the adsorption area are fed with the syrup processed by the adsorption area of the cation chromatography device (flow rate: 4 BV / h), the chromatographic columns in the regeneration area are fed with 4 wt% sodium hydroxide (flow rate: 8.5 BV / h), and the chromatographic columns in the water washing area are fed with deionized water (flow rate: 12 BV / h).

[0036] Among them, the ratio of the total mass of the cation resin in the cation simulated moving bed chromatography device to the total mass of the anion resin in the anion simulated moving bed chromatography device is 1:2.

[0037] The conductivity of the fructose syrup processed by the anion simulated moving bed chromatography device is 41.6 μs / cm, and the chromaticity is 5.5 RBU.

[0038] Compared with the discontinuous production method of connecting cation columns and anion columns in series, the continuous desalting and decolorization method in Example 1 of the present invention can increase the ion exchange efficiency of the syrup by about 20% and save about 20% of the eluent.

[0039] In the simulated moving bed chromatography system of the present invention, the adsorption area, the regeneration area, and the water washing area of the cation simulated moving bed chromatography device and the anion simulated moving bed chromatography device are reasonably divided. Considering multiple factors such as the mass ratio of cation and anion resins, the system switching time, and the flow rates in each area, the desalting and decolorization effect of the syrup, the ion exchange efficiency of the syrup, and the desalting and decolorization cost are balanced. On the basis of low cost, efficient desalting and decolorization of the syrup are achieved.

[0040] The above-described embodiments are only descriptions of the preferred modes of the present invention and do not limit the scope of the present invention. Without departing from the design spirit of the present invention, various deformations and improvements made by those of ordinary skill in the art to the technical solutions of the present invention shall fall within the protection scope determined by the claims of the present invention.

Claims

1. A method for continuous desalting and decolorizing syrup based on simulated moving bed chromatography, characterized in that: The following steps are involved: The simulated moving bed chromatography system used is composed of a cation simulated moving bed chromatography device and an anion simulated moving bed chromatography device connected in series; The cation simulated moving bed chromatography device is equipped with 20 chromatographic columns connected in series, and the areas corresponding to the 20 chromatographic columns connected in series are divided into three continuous areas connected in series: an adsorption area, a regeneration area, and a water washing area; the adsorption area is 12 chromatographic column positions, the regeneration area is 5 chromatographic column positions, and the water washing area is 3 chromatographic column positions; The adsorption zone, regeneration zone and water washing zone of the cation simulated moving bed chromatography device each have one feed port and one discharge port; The syrup to be treated is pumped into the adsorption zone of the cation simulated moving bed chromatography device. During the operation, each zone works simultaneously. When the operation time reaches the switching time, each chromatographic column in the cation simulated moving bed chromatography device moves one column position clockwise. The syrup is operated sequentially in this manner to achieve continuous operation of syrup desalting and decolorization; The anion simulated moving bed chromatography device is equipped with 20 chromatographic columns connected in series, and the areas corresponding to the 20 chromatographic columns connected in series are divided into three continuous areas connected in series: an adsorption area, a regeneration area and a water washing area; the adsorption area is 10 chromatographic column positions, the regeneration area is 6 chromatographic column positions, and the water washing area is 4 chromatographic column positions; The adsorption zone, regeneration zone and water washing zone of the anion simulated moving bed chromatography device each have one feed port and one discharge port; The syrup treated in the adsorption zone of the cation simulated moving bed chromatography device is passed into the adsorption zone of the anion simulated moving bed chromatography device. During the operation, each zone works simultaneously. When the operation time reaches the switching time, each chromatographic column in the anion simulated moving bed chromatography device moves one column position clockwise. The devices are operated sequentially in this manner to realize continuous operation of syrup desalination and decolorization, and the desalted and decolorized syrup is collected at the discharge port of the adsorption zone of the anion simulated moving bed chromatography device.

2. The method for continuous desalting and decolorizing syrup according to claim 1, characterized in that: In the cation simulated moving bed chromatography device and the anion simulated moving bed chromatography device: the feed inlet of the adsorption zone is the first chromatographic column in the clockwise direction of the zone; the feed inlet of the regeneration zone and the water washing zone is the last chromatographic column in the clockwise direction of the zone.

3. The method for continuous desalting and decolorizing syrup according to claim 1, characterized in that: The cation simulated moving bed chromatography device is filled with a cation resin; the cation resin is 001×7 or D001FD; the anion simulated moving bed chromatography device is filled with anion resin; the anion resin is D301, D354FD, ZGA355FD or ZGA352MB.

4. The method for continuous desalting and decolorizing syrup according to claim 3, characterized in that: The ratio of the total mass of the cationic resin in the cation simulated moving bed chromatography device to the total mass of the anionic resin in the anion simulated moving bed chromatography device is 1:

2.

5. The method for continuous desalting and decolorizing syrup according to claim 1, characterized in that: The operating temperature of the simulated moving bed chromatography system is 50-60° C.; the switching time is 1000s-1500s.

6. The method for continuous desalting and decolorizing syrup according to claim 1, characterized in that: For the cation simulated moving bed chromatography device: in the continuous desalting and decolorizing process, the chromatographic column located in the adsorption zone is fed with the syrup to be desalted and decolorized, the chromatographic column located in the regeneration zone is fed with 5wt% hydrochloric acid, and the chromatographic column located in the water washing zone is fed with deionized water.

7. The method for continuous desalting and decolorizing syrup according to claim 6, characterized in that: The flow rate of the syrup to be desalted and decolorized is 3-5 BV / h, the flow rate of the 5wt% hydrochloric acid is 5-10 BV / h, and the flow rate of the deionized water is 5-12 BV / h.

8. The method for continuous desalting and decolorizing syrup according to claim 1, characterized in that: For the anion simulated moving bed chromatography device: in the continuous desalting and decolorization process, the chromatographic column located in the adsorption zone is fed with the syrup treated in the adsorption zone of the cation chromatography device, the chromatographic column located in the regeneration zone is fed with 4wt% sodium hydroxide, and the chromatographic column located in the water washing zone is fed with deionized water.

9. The method for continuous desalting and decolorizing syrup according to claim 8, characterized in that: The flow rate of the treated syrup is 3-5 BV / h, the flow rate of the 4 wt % sodium hydroxide is 7-12 BV / h, and the flow rate of the deionized water is 8-15 BV / h.

10. The method for continuous desalting and decolorizing syrup according to claim 1, characterized in that: The syrup is fructose-glucose syrup; the concentration of the syrup is 10%-30%, the conductivity is 0-1000 μs / cm, and is not 0 μs / cm; the chromaticity is 0-200RBU, and is not 0RBU.