Method and system for purifying sucralose syrup

Abstract

The invention provides a method and a system for purifying sucralose syrup, and relates to the technical field of purification. The purification method comprises the following steps: decoloring sucralose syrup under normal pressure, enabling the sucralose syrup to pass through a deacidification column and an ion exchange membrane at the temperature of 15-30 DEG C at the flow rate of 0.5-2.0 cubic meters per hour, enabling the sucralose syrup to enter a deacidified syrup tank, concentrating and crystallizing, thereby obtaining the sucralose syrup. Impurities in sucralose sugar water can be removed through the Z-type ion exchange membrane and the L100-type resin, the impurity content of batch sugar water after impurity removal is reduced to 0.5-1% from original 5%, the content of sucralose is improved to 99% or above from original 95%, and the productivity of sucralose is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of purification, and in particular to a method and system for purifying sucralose syrup. Background Art

[0002] Sucralose syrup contains high levels of impurities and acetic acid. Syrup with high impurity content will lead to poor subsequent crystallization effect. The amount of mother liquor produced in each batch of syrup is large, which will cause the loss of mother liquor and reduce the production capacity of the batch of syrup.

[0003] Prior art, such as patent CN117482573A, discloses a deacidification system and deacidification method for sucralose water, wherein the deacidification system for sucralose water includes a sugar water unit, a resin kettle, and a deacidified sugar water storage unit connected in sequence; the sugar water unit is configured to store the sucralose water to be treated; the resin kettle is configured to deacidify the sucralose water using resin; the deacidified sugar water storage unit is configured to collect and store the deacidified sucralose water; the resin kettle is a stainless steel jacketed closed kettle, and a deacidification resin is arranged in the resin kettle. The method and system in the invention have high deacidification efficiency, and effectively reduce the amount of resin regeneration wastewater and the content of sucralose in the wastewater, achieving energy conservation and emission reduction, and reducing the subsequent sewage treatment costs. However, the invention is mainly aimed at the deacidification of sucralose water, and does not involve the content related to impurity removal.

[0004] Patent CN101284850A discloses a method for purifying and crystallizing sucralose, which specifically comprises the following steps: a. hydrolysis and deacetylation of sucralose-6-acetate: sucrose-6-acetate is hydrolyzed in an aqueous solution or an alcohol solution with a volume of 3-15 times the volume thereof using an alkaline catalyst to obtain an aqueous solution or an alcohol solution of sucralose; b. purification of the sucralose solution: the aqueous solution or alcohol solution of sucralose is neutralized with an acidic substance to a pH of 6-7, and then desalted using an anion-cation exchange resin or electrodialysis; c. crystallization: the aqueous solution or alcohol solution of sucralose in step b is concentrated under reduced pressure, and after concentration to no evaporation, 2-20 times the volume of a medium polar solvent is added, the temperature is raised to dissolve, a small amount of insoluble matter is filtered to remove, and then 2-5 times the volume of another weak polar solvent is added, and then more than half of the solvent is evaporated under reduced pressure, the temperature is naturally lowered by stirring, crystallization is performed, filtration is performed, and sucralose crystals are obtained by drying. The crystallization process is simple to operate, easy to control, simple in equipment, and the crystallized product has a higher purity. But this invention does not involve the relevant content of deacidification.

[0005] In view of the problems existing in the prior art, it is necessary to find a method and system for purifying sucralose water. Summary of the invention

[0006] The present invention aims to solve the problems existing in the prior art and provides a method and system for purifying sucralose water.

[0007] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0008] A method for purifying sucralose water comprises the following steps: decolorizing the sucralose water under normal pressure, passing the sucralose water through a deacidification column at a flow rate of 0.5-2.0 cubic meters per hour under 15-30° C., passing through an ion exchange membrane, entering a deacidified water tank, concentrating, and crystallizing to obtain the sucralose water.

[0009] The deacidification column is L100 type resin with a diameter-to-height ratio of 1.6:6, purchased from Anhui Liaoyuan Resin Technology Co., Ltd.

[0010] The ion exchange membrane is a Z-type ion exchange membrane with a particle size of 0.22 μm and a flow rate of 0.5-2.5 cubic meters per hour at room temperature of 25° C. and normal pressure. It was purchased from Lanran Technology Co., Ltd.

[0011] The crystallization temperature is 20°C and the crystallization time is 4-5h.

[0012] The concentration specifically includes concentration to a relative density of about 0.9-1.3 (60° C.).

[0013] The mixed solution of acetic acid and water obtained from the deacidification column enters the distillation tower, and acetic acid is obtained by vacuum distillation.

[0014] The temperature of the reduced pressure distillation is 101-105°C and the pressure is -0.075MPA.

[0015] A system for purifying the above-mentioned sucralose water comprises a water tank, a deacidification column, a Z-type ion exchange membrane, a deacidified water tank, a crystallization kettle, a distillation tower, a water receiving tank and an acetic acid receiving tank.

[0016] The sugar water tank, deacidification column, Z-type ion exchange membrane, deacidified sugar water tank and crystallization kettle are connected in series in sequence, the distillation tower is connected to the deacidification column, and the water receiving tank and acetic acid receiving tank are arranged in parallel after the distillation tower.

[0017] The technical effects achieved by the present invention are:

[0018] 1. The present invention can remove impurities in sucralose syrup through Z-type ion exchange membrane and L100 type resin, thereby reducing impurities in the syrup and improving the crystallization effect of the batch syrup, while also reducing the impurity content of the mother liquor, which reduces the crystallization of the subsequent mother liquor accumulation. The batch syrup after impurity removal has a water impurity content of 5% of the original 5% reduced to 0.5-1%. The improved batch syrup has about 0.4 cubic meters more syrup per kettle than the original, which is about 0.08 tons of sucralose, and the production capacity of sucralose is improved.

[0019] 2. The mixed solution of acetic acid and water produced by the resin cleaning of the present invention can also extract about 0.3 tons of acetic acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 Schematic diagram of the purification system of sucralose water. DETAILED DESCRIPTION

[0021] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0022] Before further describing the specific embodiments of the present invention, it should be understood that the scope of protection of the present invention is not limited to the specific embodiments described below; it should also be understood that the terms used in the examples of the present invention are for describing specific embodiments rather than for limiting the scope of protection of the present invention.

[0023] When the embodiment gives a numerical range, it should be understood that, unless otherwise specified in the present invention, the two endpoints of each numerical range and any numerical value between the two endpoints can be selected. Unless otherwise defined, all technical and scientific terms used herein have the same meanings as those of ordinary skill in the art to which the present invention belongs.

[0024] It is worth noting that the raw materials used in the present invention are all common commercially available products, so their sources are not specifically limited.

[0025] Sucralose syrup before impurity removal: about 95% sucralose, about 5% impurities, and 300-500ppm acetic acid.

[0026] Embodiment 1:

[0027] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was passed through a Z-type ion exchange membrane and L100 resin for adsorption filtration (flow rate 0.5 liters / hour) to obtain adsorbed water. The adsorbed water was sampled and analyzed for impurity content, which was about 0.6%.

[0028] Embodiment 2:

[0029] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was taken and filtered through a Z-type ion exchange membrane and L100 resin adsorption (flow rate 0.5 liters / hour) to obtain adsorbed sucrose water. The impurity content of the adsorbed sucrose water was analyzed by sampling, and the impurity content was about 0.8%.

[0030] Comparative Example 1:

[0031] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was taken and filtered through a Z-type ion exchange membrane (flow rate 0.5 liters / hour) to obtain adsorbed sucrose water. The impurity content of the adsorbed sucrose water was analyzed by sampling, and the impurity content was about 5.1%.

[0032] Comparative Example 2:

[0033] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was taken and filtered through L100 resin adsorption (flow rate 0.5 liters / hour) to obtain adsorbed sucrose water. The impurity content of the adsorbed sucrose water was analyzed by sampling, which was about 4.6%.

[0034] Comparative Example 3:

[0035] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was directly filtered (flow rate 0.5 liters / hour) to obtain the filtered water. The impurity content of the filtered water was analyzed and was about 6.2%.

[0036] Comparative Example 4:

[0037] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was directly filtered (flow rate 0.5 liters / hour) to obtain the filtered water. The impurity content of the filtered water was analyzed and was about 5.7%.

[0038] Comparative Example 5:

[0039] In the experiment under normal temperature and pressure conditions, 3 liters of sucralose water was directly filtered (flow rate 0.5 liters / hour) to obtain the filtered water. The impurity content of the filtered water was analyzed by sampling, which was about 5.4%.

[0040] Effect detection:

[0041] Detection method: Liquid chromatography and atomic absorption spectrometry were used to detect the impurity content, acetic acid content and sucralose content. The test results are shown in Table 1 below.

[0042] Table 1

[0043] Examples Impurity content Acetic acid content Sucralose content Example 1 0.6％ 128ppm 99.4％ Example 2 0.8％ 121ppm 99.2％ Comparative Example 1 5.1％ 234ppm 94.9％ Comparative Example 2 4.6％ 216ppm 95.4％ Comparative Example 3 6.2％ 302ppm 93.8％ Comparative Example 4 5.7％ 268ppm 94.3％ Comparative Example 5 5.4％ 254ppm 94.6％

[0044] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

[0045] In summary, the impurities in sucralose syrup can be removed by Z-type ion exchange membrane and L100 resin, thereby reducing the impurities in the syrup and improving the crystallization effect of the batch syrup. At the same time, the impurity content of the mother liquor is also reduced, which reduces the crystallization of the subsequent mother liquor accumulation and improves the production capacity of sucralose.

Claims

1. A method for purifying sucralose syrup, characterized in that: The following steps are involved: Under normal pressure, sucralose water is decolorized, passed through a deacidification column at a flow rate of 0.5-2.0 cubic meters per hour at 15-30°C, passed through an ion exchange membrane, and entered into a deacidified sugar water tank, where it is concentrated and crystallized to obtain the product.

2. The purification method according to claim 1, characterized in that: The deacidification column is L100 type resin with a diameter-to-height ratio of 1.6:

6.

3. The purification method according to claim 1, characterized in that: The ion exchange membrane is a Z-type ion exchange membrane, the particle size of the Z-type ion exchange membrane is 0.22 microns, and the flow rate is 0.5-2.5 cubic meters per hour at room temperature 25° C. and normal pressure.

4. The purification method according to claim 1, characterized in that: The crystallization temperature is 20°C and the crystallization time is 4-5h.

5. The purification method according to claim 1, characterized in that: The concentration specifically includes concentration to a relative density of about 0.9-1.3 (60° C.).

6. The purification method according to claim 1, characterized in that: The mixed solution of acetic acid and water obtained from the deacidification column enters the distillation tower, and acetic acid is obtained by vacuum distillation.

7. The purification method according to claim 6, characterized in that: The temperature of the reduced pressure distillation is 101-105°C and the pressure is -0.075MPA.

8. A system for purifying sucralose water for implementing the extraction method according to any one of claims 1 to 7, characterized in that: The invention comprises a sugar water tank, a deacidification column, a Z-type ion exchange membrane, a sugar water tank after deacidification, a crystallization kettle, a distillation tower, a water receiving tank and an acetic acid receiving tank.

9. The purification system according to claim 8, characterized in that: The sugar water tank, deacidification column, Z-type ion exchange membrane, deacidified sugar water tank and crystallization kettle are connected in series in sequence, the distillation tower is connected to the deacidification column, and the water receiving tank and acetic acid receiving tank are arranged in parallel after the distillation tower.

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