AU2016347128B2 - Apparatus and method for recovering residual sugar in cane sugar manufacturing process - Google Patents

Apparatus and method for recovering residual sugar in cane sugar manufacturing process Download PDF

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AU2016347128B2
AU2016347128B2 AU2016347128A AU2016347128A AU2016347128B2 AU 2016347128 B2 AU2016347128 B2 AU 2016347128B2 AU 2016347128 A AU2016347128 A AU 2016347128A AU 2016347128 A AU2016347128 A AU 2016347128A AU 2016347128 B2 AU2016347128 B2 AU 2016347128B2
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membrane module
ultrafiltration
nanofiltration
diafiltration
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AU2016347128A1 (en
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Xiangrong Chen
Xiaofeng HANG
Jianquan LUO
Yinhua Wan
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Institute of Process Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration

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Abstract

An apparatus and a method for recovering residual sugar in a cane sugar manufacturing process. The apparatus comprises a multi-stage countercurrent filtration-washing unit and a nanofiltration-concentrating unit, the multi-stage countercurrent filtration-washing unit comprising ultrafiltration membrane components in at least two stages, and the nanofiltration-concentrating unit comprising a nanofiltration membrane component; an outlet at the retentate side of the previous-stage ultrafiltration membrane component of the multi-stage countercurrent filtration-washing unit being connected to an inlet at the retentate side of the next-stage ultrafiltration membrane component, an inlet at the retentate side of the previous-stage ultrafiltration membrane component being connected to an outlet at the permeate side of the next-stage ultrafiltration membrane component; and an outlet at the permeate side of the first-stage ultrafiltration membrane component of the multi-stage countercurrent filtration-washing unit being connected to an inlet at the retentate side of the nanofiltration membrane component. Said apparatus can ensure the loss ratio of the cane sugar to be less than 2% in a decolorizing section, save 50% or more of the filtration-washing water consumption, and obtain filtration-washing permeate with high sugar concentration. The operation is easy and safe, production can be continuous, and the obtained sugar-containing concentrate is free of chemical additives.

Description

APPARATUS AND METHOD FOR RECOVERING RESIDUAL SUGAR IN CANE SUGAR MANUFACTURING PROCESS
Technical Field
The present invention belongs to the technical field of sugar manufacturing, and relates to a device and a method for recovering residual sugar in the membrane-based process of manufacturing sugar from sugarcane, in particular relates to a device and a method for recovering residual sugar in the process of manufacturing sugar from sugarcane by using a multi-stage countercurrent diafiltration manner.
Background
The existing processes of manufacturing sugar from sugarcane comprise sections such as sugarcane pretreatment, juice extraction, cane juice clarification, scouring, etc. The clarification effects of cane juice directly determine the quality of sugar product. In traditional processes, a large amount of lime and sulfur dioxide (sulfitation process) are added, or lime and carbonic acid gas (carbonatation process) are added to the mixed juice, followed by separation of the precipitate to remove non-sugar impurities in the mixed juice to reduce colourity and turbidity in order to obtain clear syrup juice. Therefore, a large amount of waste water and solid waste are generated in sugar manufacturing processes, and there are problems such as complicated processes, low decolorization rate, unstable quality of the sugar product, and the like. At present, in cane sugar factories of China, especially sugar factories using sulfitation processes, the product quality is always affected and the product may even be degraded or become substandard sugar since the two indicators, colourity and turbidity exceed the standards.
Due to the above problems presented in the existing processes of manufacturing sugar from sugarcane, many new methods such as ion exchange method, electrodialysis
EX180270PPC-AU method, and membrane method have gradually been concerned and researched. CN 103194545B discloses a method for processing mixed sugarcane clear juice by using a membrane method, comprising the following steps: (1) mixed clear juice was filtered through a first-stage ultrafiltration membrane, then the resulting clear juice was filtered through a second-stage ultrafiltration membrane, the concentrated solution obtained after filtration by the first-stage ultrafiltration membrane was used to evaporate to manufacture sugar, the concentrated solution obtained after filtration by the second-stage ultrafiltration membrane was combined with the mixed clear juice to filter through the first-stage ultrafiltration membrane; (2) the thin solution obtained after filtration by the second-stage ultrafiltration membrane in step (1) was concentrated in a membrane concentration device to obtain concentrated solution and thin water; the first-stage ultrafiltration membrane had a molecular weight cut-off of 50,000-100,000 daltons, and the second-stage ultrafiltration membrane had a molecular weight cut-off of 1,000-20,000 daltons. This method comprises two stages of ultrafiltration clarification decolorization and one stage of reverse osmosis concentration dehydration. However, due to certain retention effect of ultrafiltration on sucrose, the concentrated solution obtained after the two stages of ultrafiltration contained high concentrations of sucrose and the recovery rate of sucrose was generally only 60-70%, resulting in a great residual sugar loss. Both CN102659855A and CN103710470A disclose a method for decolorizing sugar juice by combining membrane separation with ion exchange, but none of them mentioned the problem of residual sugar recovery in the concentrated solution or the eluted concentrated solution. CN 201510486534.4 recites that the concentrated solution in decolorization section was treated with chemicals such as lime or sulfur dioxide, and then returned to clarification section. However, this process still did not get rid of the traditional chemical method, resulting in a contamination of molasses, reducing its added value.
The diafiltration operation is a key technology during the membrane separation process, mainly used for desalination and to increase product purity. The diafiltration operation comprises an equal-volume continuous diafiltration and a variable-volume
EX180270PPC-AU intermittent diafiltration (also called dilution-concentration). The former has high diafiltration efficiency and is easy to operate continuously; the latter has a large diafiltration flux, however, it consumes a large amount of water and requires an additional buffer tank.
The use of continuous diafiltration to recover residual sugar in the membrane-based process of manufacturing sugar from sugarcane still requires further studies.
Summary of the Invention
In view of the deficiencies in the prior art, the object of the present invention is to provide a device and a method for recovering residual sugar in the membrane-based process of manufacturing sugar from sugarcane. The device can not only recover most of residual sugar in the sucrose refining process, but also reduce the amount of water consumed in diafiltration. In addition, the device is easy and safe to operate, easy to produce continuously, and there is free of chemical additives in the resulting sugar-containing concentrated solution.
To achieve this object, the present invention adopts the following technical solutions:
the first object of the present invention is to provide a device for recovering residual sugar in the membrane-based process of manufacturing sugar from sugarcane, which comprises a multi-stage countercurrent diafiltration unit and a nanofiltration concentration unit, the multi-stage countercurrent diafiltration unit comprises at least 2 stages of ultrafiltration membrane modules, the nanofiltration concentration unit comprises a nanofiltration membrane module;
the outlet on the retentate side of the previous-stage ultrafiltration membrane module of the multi-stage countercurrent diafiltration unit is connected to the inlet on the retentate side of the next-stage ultrafiltration membrane module, the inlet on the retentate side of the previous-stage ultrafiltration membrane module is connected to
EX180270PPC-AU the outlet on the permeation side of the next-stage ultrafiltration membrane module;
the outlet on the permeation side of the first-stage ultrafiltration membrane module of the multi-stage countercurrent diafiltration unit is connected to the inlet on the retentate side of the nanofiltration membrane module;
a sugar-containing concentrated solution is obtained on the retentate side of the nanofiltration membrane module, and a pigment-containing retentate is obtained on the retentate side of the last-stage ultrafiltration membrane module of the multi-stage countercurrent diafiltration unit.
The device is mainly used for recovering residual sugar in the process of manufacturing sugar using a membrane method, and can also be used for recovering residual sugar in the process of manufacturing sugar using other methods.
The recovery device uses a multi-stage countercurrent diafiltration technology to achieve the separation of sucrose and non-sugar substances in the residual sugar solution, reducing the residual sugar loss in the sucrose refining process using a membrane method, and increasing the recovery rate of sucrose in the entire clarification decolorization section, thereby reducing the production costs of sucrose.
The outlet on the permeation side of the nanofiltration membrane module is connected to the inlet on the retentate side of the last-stage nanofiltration membrane module of the multi-stage countercurrent diafiltration unit, so as to achieve water recycling and greatly save the water used for diafiltration.
Preferably, the diafiltration manner of the multi-stage countercurrent diafiltration unit is equal-volume countercurrent diafiltration. The equal-volume countercurrent diafiltration is to pump water for diafiltration into the last-stage ultrafiltration membrane module continuously, controlling the water adding rate to be equivalent to the permeation flux of the ultrafiltration membrane module, so that the retentate
EX180270PPC-AU volume of the diafiltration of each stage is maintained.
The multi-stage countercurrent diafiltration unit is used for removing macromolecular impurities presented in the sugar-containing solution. The multi-stage countercurrent diafiltration unit comprises 2-5 stages of ultrafiltration membrane modules, such as 2 stages of ultrafiltration membrane modules, 3 stages of ultrafiltration membrane modules, 4 stages of ultrafiltration membrane modules or 5 stages of ultrafiltration membrane modules.
Preferably, the ultrafiltration membrane module has a molecular weight cut-off of 1000-5000 Da, such as 1500 Da, 2000 Da, 2500 Da, 3000 Da, 3500 Da, 4000 Da, or 4500 Da, etc.
Preferably, the ultrafiltration membrane module has an operating temperature of 25-95 °C, such as 30 °C, 40 °C, 50 °C, 60 °C, 65 °C, 70 °C, 80 °C, 90 °C, or 95 °C, etc.
Preferably, the ultrafiltration membrane module has an operating pressure of 0.5-1.5 MPa, such as 0.6 MPa, 0.8 MPa, 1.0 MPa, 1.2 MPa, 1.3 MPa, or 1.4 MPa, etc.
Preferably, the ultrafiltration membrane module is in a spiral, tubular, flat, or hollow fiber form.
Preferably, the material of the ultrafiltration membrane module is polysulfone, polyether sulfone, sulfonated polyether sulfone or polyvinylidene fluoride.
The ultrafiltration membrane modules of each stage of the multi-stage countercurrent diafiltration unit can be composed of one or more ultrafiltration membrane modules connected in parallel, such as composed of 2, 3, 4, 6, or 8 ultrafiltration membrane modules connected in parallel. Those skilled in the art can select an appropriate number of ultrafiltration membrane modules according to the actual flow rate.
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The nanofiltration concentration unit is used to further concentrate the sugar-containing solution obtained from the multi-stage countercurrent diafiltration unit, and the nanofiltration membrane module is in the form of spiral membrane.
The nanofiltration membrane module can be composed of one or more nanofiltration membrane modules connected in parallel, such as composed of 2, 3, 4, 6, or 8 nanofiltration membrane modules connected in parallel. Those skilled in the art can select an appropriate number of nanofiltration membrane modules according to the actual flow rate.
Preferably, the nanofiltration membrane module has a membrane molecular weight cut-off of 90-400 Da, such as 100 Da, 120 Da, 150 Da, 200 Da, 250 Da, 300 Da, or 350 Da, etc, preferably 200 Da.
Preferably, the nanofiltration membrane module has an operating temperature of 25-95 °C, such as 30 °C, 40 °C, 50 °C, 60 °C, 70 °C, 80 °C or 90 °C, etc.
Preferably, the nanofiltration membrane module has an operating pressure of 2.0-4.1 MPa, such as 2.2 MPa, 2.5 MPa, 2.8 MPa, 3.0 MPa, 3.2 MPa, 3.5 MPa, 3.8 MPa, or 4.0 MPa, etc.
The second object of the present invention is to provide a method for recovering residual sugar by using the device as described above, which comprises the following steps:
(1) subjecting a sugar-containing solution to multi-stage countercurrent ultrafiltration to obtain a permeated solution of the first-stage ultrafiltration and a retentate of the last-stage ultrafiltration, and discharging the retentate of the last-stage ultrafiltration;
(2) subjecting the permeated solution of the first-stage ultrafiltration to nanofiltration concentration to obtain a sugar-containing concentrated solution and a permeated solution of the nanofiltration .
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In the method for recovering residual sugar provided by the present invention, the permeated solution produced in each stage of the diafiltration can in turn be used as water for diafiltration for the previous-stage. The permeated solution of the first-stage diafiltration has high sugar concentration and can be directly subjected to the nanofiltration concentration section to produce water for diafiltration, thus the water consumption is greatly saved, and the energy consumption in the nanofiltration concentration section and the evaporation and crystallization section is greatly reduced. The method is easy to produce continuously and free of chemical additives.
The sugar-containing solution in step (1) is a concentrated solution of mixed sugarcane juice, which has been concentrated 10-30 times, such as 12 times, 15 times, 20 times, 22 times, 25 times or 28 times, by microfiltration pretreatment and ultrafiltration decoloration treatment.
Preferably, the manner of the multi-stage countercurrent ultrafiltration in step (1) is equal-volume countercurrent diafiltration.
Preferably, the water used for diafiltration in the multi-stage countercurrent ultrafiltration in step (1) is deionized water.
Preferably, the volume of the water used for diafiltration in the multi-stage countercurrent diafiltration unit in step (1) is 1-3 times, such as 1 time, 2 times or 3 times of the volume of the sugar-containing solution.
Preferably, the retentate of the last-stage ultrafiltration in step (1) is used to extract natural pigments.
The multi-stage countercurrent ultrafiltration in step (1) is performed by 2-5 stages of ultrafiltration membrane modules, for example, the countercurrent ultrafiltration is performed by 2 stages of ultrafiltration membrane modules, 3 stages of ultrafiltration membrane modules, 4 stages of ultrafiltration membrane modules or 5 stages of
EX180270PPC-AU ultrafiltration membrane modules.
Preferably, the ultrafiltration membrane module has a molecular weight cut-off of 1000-5000 Da, such as 1500 Da, 2000 Da, 2500 Da, 3000 Da, 3500 Da, 4000 Da, or 4500 Da, etc.
Preferably, the ultrafiltration membrane module has an operating temperature of 25-95 °C, such as 30 °C, 40 °C, 50 °C, 60 °C, 65 °C, 70 °C, 80 °C, 90 °C, or 95 °C, etc.
Preferably, the ultrafiltration membrane module has an operating pressure of 0.5-1.5
MPa, such as 0.6 MPa, 0.8 MPa, 1.0 MPa, 1.2 MPa, 1.3 MPa, or 1.4 MPa, etc.
Preferably, the ultrafiltration membrane module is in a spiral, tubular, flat, or hollow fiber form.
Preferably, the material of the ultrafiltration membrane module is polysulfone, polyether sulfone, sulfonated polyether sulfone or polyvinylidene fluoride.
The nanofiltration concentration of step (2) is performed by a nanofiltration membrane module.
Preferably, the nanofiltration membrane module has a membrane molecular weight cut-off of 90-400 Da, such as 100 Da, 120 Da, 150 Da, 200 Da, 250 Da, 300 Da, or 350 Da, etc, preferably 200 Da.
Preferably, the nanofiltration membrane module has an operating temperature of 25-95 °C, such as 30 °C, 40 °C, 50 °C, 60 °C, 70 °C, 80 °C or 90 °C, etc.
Preferably, the nanofiltration membrane module has an operating pressure of 2.0-4.1
MPa, such as 2.2 MPa, 2.5 MPa, 2.8 MPa, 3.0 MPa, 3.2 MPa, 3.5 MPa, 3.8 MPa, or 4.0 MPa, etc.
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Preferably, the nanofiltration membrane module is in the form of spiral membrane.
Preferably, the sugar-containing concentrated solution of step (2) is crystallized by evaporation to obtain sugar.
The permeated solution of the nanofiltration in step (2) is used as water for diafiltration for the multi-stage countercurrent ultrafiltration in step (1).
Preferably, the volume ratio of the permeated solution of the nanofiltration in step (2) to the water for diafiltration for the multi-stage countercurrent ultrafiltration in step (1) is between 2:3-1:5, such as 4:15, 1:3, 7:15 or 3:5, etc.
By using the permeated solution of the nanofiltration as water for diafiltration for the multi-stage countercurrent ultrafiltration, the water consumption can be greatly reduced.
As a preferred technical solution, the method for recovering residual sugar comprises the following steps:
(1) subjecting a sugar-containing solution to multi-stage countercurrent ultrafiltration to obtain a permeated solution of the first-stage ultrafiltration and a retentate of the last-stage ultrafiltration, and discharging the retentate of the last-stage ultrafiltration, the multi-stage countercurrent ultrafiltration is performed by 2-5 stages of ultrafiltration membrane modules, the ultrafiltration membrane module has a molecular weight cut-off of 1000-5000 Da, an operating temperature of 25-95 °C, and an operating pressure of 0.5-1.5 MPa;
(2) subjecting the permeated solution of the first-stage ultrafiltration to nanofiltration concentration to obtain a sugar-containing concentrated solution and a permeated solution of the nanofiltration, the nanofiltration concentration is performed by a nanofiltration membrane module, the nanofiltration membrane module has a membrane molecular weight cut-off of 90-400 Da, an operating temperature of
EX180270PPC-AU
25-95 °C and an operating pressure of 2.0-4.1 MPa;
(3) using the permeated solution of the nanofiltration and the deionized water in a volume ratio of 2:1-1:4 as water for diafiltration for the multi-stage countercurrent ultrafiltration in step (1).
Compared with the prior art, the present invention has the following beneficial effects:
1. The device for recovering residual sugar in the process of manufacturing sugar from sugarcane provided by the present invention is easy and safe to operate, easy to produce continuously, and there is free of chemical additive in the recovered sugar.
2. The method for recovering residual sugar in the process of manufacturing sugar from sugarcane provided by the present invention not only reduces the residual sugar loss during ultrafiltration decolorization of mixed sucrose juice, but also saves water consumption by more than 50%, ensuring that the loss rate of sucrose in the decolorization section is less than 2% and a permeated solution of the diafiltration with high sugar concentration is obtained.
3. In the device for recovering residual sugar in the process of manufacturing sugar from sugarcane provided by the present invention, the retentate obtained in the last-stage ultrafiltration membrane module has extremely low sugar content and is free of chemicals, and can be used to extract natural pigments.
Description of the Drawings
Figure. 1 is a structural schematic view of the device for recovering residual sugar in the process of manufacturing sugar from sugarcane provided in Example 1.
Detailed Description
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The technical solutions of the present invention will be further described below with reference to the accompanying drawings and specific embodiments. The protection scope of the subject matter of the present invention is not limited to these examples.
Example 1
A device for recovering residual sugar in the process of manufacturing sugar from sugarcane is shown in Figure 1. The device comprised a multi-stage countercurrent diafiltration unit and a nanofiltration concentration unit. The multi-stage countercurrent diafiltration unit comprised three stages of ultrafiltration membrane modules, and the three-stage ultrafiltration membrane module was a first-stage, a second-stage and a third-stage ultrafiltration membrane module which were connected by pipelines successively; the nanofiltration concentration unit was a nanofiltration membrane module;
The ultrafiltration membrane modules were 4040-type, food-grade, spiral, polyether sulfone membrane modules. The first-stage ultrafiltration membrane module was formed of 6 membrane modules connected in parallel, the second-stage ultrafiltration membrane module was formed of 4 membrane modules connected in parallel and the third-stage ultrafiltration membrane module was formed of 2 membrane modules connected in parallel; the nanofiltration membrane module was food-grade, 4040-type, spiral, organic membrane module and was formed of 2 membrane modules connected in parallel;
The outlet on the retentate side of the first-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the second-stage ultrafiltration membrane module through a pipeline, the outlet on the retentate side of the second-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the third-stage ultrafiltration membrane module; the outlet on the permeation side of the third-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the second-stage ultrafiltration membrane module, the 11
EX180270PPC-AU outlet on the permeation side of the second-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the first-stage ultrafiltration membrane module;
The outlet on the permeation side of the first-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the nanofiltration membrane module through a pipeline, the outlet on the permeation side of the nanofiltration membrane module was connected to the inlet on the retentate side of the third-stage ultrafiltration membrane module;
A sugar-containing concentrated solution was obtained on the retentate side of the nanofiltration membrane module, which was crystallized by evaporation to obtain sugar; and the retentate obtained from the third-stage ultrafiltration membrane module was discharged to extract natural pigments.
Example 2
A device for recovering residual sugar in the process of manufacturing sugar from sugarcane comprised a multi-stage countercurrent diafiltration unit and a nanofiltration concentration unit. The multi-stage countercurrent diafiltration unit comprised two stages of ultrafiltration membrane modules, and the two-stage ultrafiltration membrane module was a first-stage and a second-stage ultrafiltration membrane module which were connected by pipelines successively; the nanofiltration concentration unit was a nanofiltration membrane module;
The ultrafiltration membrane modules were hollow fiber, polyvinylidene chloride membrane module. Both the first-stage ultrafiltration membrane module and the second-stage ultrafiltration membrane module were formed of 4 membrane modules connected in parallel; the nanofiltration membrane module was food-grade, 4040-type, spiral, organic membrane module and was formed of 2 membrane modules connected in parallel;
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The outlet on the retentate side of the first-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the second-stage ultrafiltration membrane module through a pipeline, the outlet on the retentate side of the second-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the first-stage ultrafiltration membrane module;
The outlet on the permeation side of the first-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the nanofiltration membrane module through a pipeline, the outlet on the permeation side of the nanofiltration membrane module was connected to the inlet on the retentate side of the second-stage ultrafiltration membrane module;
A sugar-containing concentrated solution was obtained on the retentate side of the nanofiltration membrane module, which was crystallized by evaporation to obtain sugar; and the retentate obtained from the second-stage ultrafiltration membrane module was discharged to extract natural pigments.
Example 3
A device for recovering residual sugar in the process of manufacturing sugar from sugarcane comprised a multi-stage countercurrent diafiltration unit and a nanofiltration concentration unit. The multi-stage countercurrent diafiltration unit comprised five stages of ultrafiltration membrane modules, and the five-stage ultrafiltration membrane module was a first-stage, a second-stage, a third-stage, a fourth-stage and a fifth-stage ultrafiltration membrane module which were connected by pipelines successively; the nanofiltration concentration unit was a nanofiltration membrane module;
The ultrafiltration membrane modules were flat, sulfonated polyether sulfone membrane module. All of the first-stage to fifth-stage ultrafiltration membrane modules were formed of 3 membrane modules connected in parallel; the
EX180270PPC-AU nanofiltration membrane module was food-grade, 4040-type, spiral, organic membrane module and was formed of 4 membrane modules connected in parallel;
The outlet on the retentate side of the first-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the second-stage ultrafiltration membrane module through a pipeline, the outlet on the retentate side of the second-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the third-stage ultrafiltration membrane module, the outlet on the retentate side of the third-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the fourth-stage ultrafiltration membrane module, the outlet on the retentate side of the fourth-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the fifth-stage ultrafiltration membrane module; the outlet on the permeation side of the fifth-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the fourth-stage ultrafiltration membrane module, the outlet on the permeation side of the fourth-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the third-stage ultrafiltration membrane module, the outlet on the permeation side of the third-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the second-stage ultrafiltration membrane module, the outlet on the permeation side of the second-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the first-stage ultrafiltration membrane module;
The outlet on the permeation side of the first-stage ultrafiltration membrane module was connected to the inlet on the retentate side of the nanofiltration membrane module through a pipeline, the outlet on the permeation side of the nanofiltration membrane module was connected to the inlet on the retentate side of the fifth-stage ultrafiltration membrane module;
A sugar-containing concentrated solution was obtained on the retentate side of the nanofiltration membrane module, which was crystallized by evaporation to obtain
EX180270PPC-AU sugar; and the retentate obtained from the fifth-stage ultrafiltration membrane module was discharged to extract natural pigments.
Example 4
Residual sugar was recovered by using the recovery device described in Example 1, and the following steps are comprised:
Firstly, the three-stage countercurrent diafiltration unit was filled with deionized water to start the diafiltration system. The ultrafiltration membrane modules of the three-stage countercurrent diafiltration unit had a molecular weight cut-off of 2000 Da, an operating temperature of 60 °C and an operating pressure of 1.0 MPa. Then the concentrated solution (with a sucrose content of 15%, the sucrose content in the mixed sugarcane juice stoste was 10%) of mixed sugarcane juice, which had been concentrated 20 times by microfiltration pretreatment and ultrafiltration decolorization, was pumped into the three-stage countercurrent diafiltration unit at a flow rate of 0.25 t/h. At the same time, deionized water was added to the third-stage ultrafiltration membrane module at a flow rate of 0.25 t/h. The permeated solution of diafiltration obtained from the first-stage ultrafiltration membrane module was pumped into the nanofiltration membrane module at a flow rate of 0.5 t/h. The nanofiltration membrane module had a molecular weight cut-off of 250 Da, an operating temperature of 60 °C, an operating pressure of 3.0 MPa and a concentration multiple of 2. A permeated solution of nanofiltration at a flow rate of 0.25 t/h was produced to be used as part of the water for diafiltration of the third-stage ultrafiltration membrane module. The total flow rate of the water for diafiltration of the third-stage ultrafiltration membrane module was 0.5 t/h, and at the same time, a permeated solution of the third-stage diafiltration at a flow rate of 0.5 t/h was produced to be used as water for diafiltration of the second-stage ultrafiltration membrane module, and a permeated solution of the second-stage diafiltration at a flow rate of 0.5 t/h was produced to be used as water for diafiltration of the first-stage.
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When the system was stable, the sugar content in the residual solution of the third-stage diafiltration was approximately 2.32%, the sucrose content in the concentrated solution of the nanofiltration was approximately 12.6% with a colourity of 798 IU, and the recovery rate for residual sugar was 84.5%, the residual sugar loss accounted for 1.16% of the total sugar of the entire process, and the decolorization rate of the recovered concentrated solution of the nanofiltration was 96%.
The water consumption of a conventional dilution-concentration intermittent diafiltration (the diafiltration membrane module was a spiral polyether sulfone membrane module, with a molecular weight cut-off of 2000 Da, an operating temperature of 60 °C, a pressure of 1.0 MPa and a dilution multiple of 2) to obtain a same residual sugar recovery rate was about 4 times that of the new process, the decolorization rate was reduced to 92%, and the sugar content in the permeated solution of the ultrafiltration diafiltration was only 3.17%.
By using the recovery device described in Example 1, water was saved by 75%, the decolorization rate was increased by 4.3%, and the sugar concentration in the recovered permeated solution of the diafiltration was increased by 297%.
A comparison of the parameters in the residual sugar recovery process by using the recovery device described in Example 1 and a conventional dilution-concentration intermittent diafiltration is shown in Table 1.
Table 1. Comparison of the amount of water for diafiltration consumed in different diafiltration methods and product indicators
diafiltration methods and dilution-concentration equal-volume
indicators intermittent countercurrent
diafiltration continuous diafiltration
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amount of water for diafiltration (t/h) 1 0.25
yield of the decolourized solution after diafiltration/concentration (t/h) 1 0.25
sucrose content in the decolourized solution after diafiltration/concentration (%) 3.17 12.6
colourity of the decolourized solution after diafiltration/concentration (IU) 1596 798
Example 5
Residual sugar was recovered by using the recovery device described in Example 1, and the following steps are comprised:
Firstly, the three-stage countercurrent diafiltration unit was filled with deionized water to start the system. The ultrafiltration membrane modules of the three-stage countercurrent diafiltration unit had a molecular weight cut-off of 1500 Da, an operating temperature of 65 °C and an operating pressure of 0.8 MPa. Then the concentrated solution (with a sucrose content of 16%, the sucrose content in the mixed sugarcane juice stoste was 11%) of mixed sugarcane juice, which had been concentrated 20 times by microfiltration pretreatment and ultrafiltration decolorization, was pumped into the three-stage countercurrent diafiltration unit at a
EX180270PPC-AU flow rate of 0.25 t/h. At the same time, deionized water was added to the third-stage ultrafiltration membrane module at a flow rate of 0.5 t/h. The permeated solution of diafiltration obtained from the first-stage diafiltration was pumped into the nanofiltration membrane module at a flow rate of 0.75 t/h. The nanofiltration membrane module had a molecular weight cut-off of 200 Da, the nanofiltration concentration had an operating temperature of 55 °C, an operating pressure of 3.2 MPa and a concentration multiple of 1.5. A permeated solution of nanofiltration at a flow rate of 0.25 t/h was produced to be used as part of the water for diafiltration of the third-stage ultrafiltration membrane module. The total flow rate of the water for diafiltration of the third-stage ultrafiltration membrane module was 0.75 t/h, and at the same time, a permeated solution of the third-stage diafiltration at a flow rate of 0.75 t/h was produced to be used as water for diafiltration of the second-stage, and a permeated solution of the second-stage diafiltration at a flow rate of 0.75 t/h was produced to be used as water for diafiltration of the first-stage.
When the system was stable, the sugar content in the residual solution of the third-stage diafiltration was approximately 1.12%, the sucrose content in the concentrated solution of the nanofiltration was approximately 7.41% with a colourity of 848 IU, and the recovery rate for residual sugar was 92.6%, the residual sugar loss accounted for 0.5% of the total sugar of the entire process, and the decolorization rate of the recovered concentrated solution of the nanofiltration was 94%.
The water consumption of a conventional dilution-concentration intermittent diafiltration (the diafiltration membrane module was a spiral polyether sulfone membrane module, with a molecular weight cut-off of 1500 Da, an operating temperature of 65 °C, a pressure of 0.8 MPa and a dilution multiple of 2) to obtain a same residual sugar recovery rate was about 3 times that of the new process, the decolorization rate was reduced to 88%, and the sugar content in the decolourized solution of the diafiltration was only 2.48%.
EX180270PPC-AU
By using the recovery device described in Example 1, water was saved by 66.7%, the decolorization rate was increased by 6.8%, and the sugar concentration in the recovered permeated solution of the diafiltration was increased by 199%.
A comparison of the parameters in the residual sugar recovery process by using the recovery device described in Example 1 and a conventional dilution-concentration intermittent diafiltration is shown in Table 2.
Table 2. Comparison of the amount of water for diafiltration consumed in different diafiltration methods and product indicators
diafiltration methods and indicators dilution-concentration intermittent diafiltration equal-volume countercurrent continuous diafiltration
amount of water for diafiltration (t/h) 1.5 0.5
yield of the decolourized solution after diafiltration/concentration (t/h) 1.5 0.5
sucrose content in the decolourized solution after diafiltration/concentration (%) 2.48 7.41
EX180270PPC-AU
colourity of the decolourized solution after diafiltration/concentration (IU) 1696 848
Example 6
Residual sugar was recovered by using the recovery device described in Example 1, and the following steps are comprised:
Firstly, the three-stage countercurrent diafiltration unit was filled with deionized water to start the system. The ultrafiltration membrane modules of the three-stage countercurrent diafiltration unit had a molecular weight cut-off of 1000 Da, an operating temperature of 95 °C and an operating pressure of 1.5 MPa. Then the concentrated solution (with a sucrose content of 16%, the sucrose content in the mixed sugarcane juice stoste was 10%) of mixed sugarcane juice, which had been concentrated 30 times by microfiltration pretreatment and ultrafiltration decolorization, was pumped into the three-stage countercurrent diafiltration unit at a flow rate of 0.25 t/h. At the same time, deionized water was added to the third-stage ultrafiltration membrane module at a flow rate of 0.4 t/h. The permeated solution of diafiltration obtained from the first-stage diafiltration was pumped into the nanofiltration membrane module at a flow rate of 0.5 t/h. The nanofiltration membrane module had a molecular weight cut-off of 90 Da, the nanofiltration concentration had an operating temperature of 95 °C, an operating pressure of 4.1 MPa and a concentration multiple of 1.25. A permeated solution of nanofiltration at a flow rate of 0.1 t/h was produced to be used as part of the water for diafiltration of the third-stage ultrafiltration membrane module. The total flow rate of the water for diafiltration of the third-stage ultrafiltration membrane module was 0.5 t/h, and at the same time, a permeated solution of the third-stage diafiltration at a flow rate of 0.5 t/h was produced to be used as water for diafiltration of the second-stage, and a
EX180270PPC-AU permeated solution of the second-stage diafiltration at a flow rate of 0.5 t/h was produced to be used as water for diafiltration of the first-stage.
When the system was stable, the sugar content in the residual solution of the third-stage diafiltration was approximately 2.82%, the sucrose content in the concentrated solution of the nanofiltration was approximately 8.2% with a colourity of 736 IU, and the recovery rate for residual sugar was 82%, the residual sugar loss accounted for 0.9% of the total sugar of the entire process, and the decolorization rate of the recovered concentrated solution of the nanofiltration was 94.8%.
The water consumption of a conventional dilution-concentration intermittent diafiltration (the diafiltration membrane module was a spiral polyether sulfone membrane module, with a molecular weight cut-off of 1000 Da, an operating temperature of 95 °C, a pressure of 1.5 MPa and a dilution multiple of 2) to obtain a same residual sugar recovery rate was about 3 times that of the new process, the decolorization rate was reduced to 89%, and the sugar content in the decolourized solution of the diafiltration was only 2.75%.
By using the recovery device described in Example 1, water was saved by 66.7%, the decolorization rate was increased by 6.5%, and the sugar concentration in the recovered permeated solution of the diafiltration was increased by 198%.
Example 7
Residual sugar was recovered by using the recovery device described in Example 1, and the following steps are comprised:
Firstly, the three-stage countercurrent diafiltration unit was filled with deionized water to start the system. The ultrafiltration membrane modules of the three-stage countercurrent diafiltration unit had a molecular weight cut-off of 5000 Da, an operating temperature of 25 °C and an operating pressure of 0.5 MPa. Then the
EX180270PPC-AU concentrated solution (with a sucrose content of 14%, the sucrose content in the mixed sugarcane juice stoste was 11%) of mixed sugarcane juice, which had been concentrated 10 times by microfiltration pretreatment and ultrafiltration decolorization, was pumped into the three-stage countercurrent diafiltration unit at a flow rate of 0.25 t/h. At the same time, deionized water was added to the third-stage ultrafiltration membrane module at a flow rate of 0.25 t/h. The permeated solution of diafiltration obtained from the first-stage diafiltration was pumped into the nanofiltration membrane module at a flow rate of 0.5 t/h. The nanofiltration membrane module had a molecular weight cut-off of 400 Da, the nanofiltration concentration had an operating temperature of 25 °C, an operating pressure of 2.0 MPa and a concentration multiple of 2. A permeated solution of nanofiltration at a flow rate of 0.25 t/h was produced to be used as part of the water for diafiltration of the third-stage ultrafiltration membrane module. The total flow rate of the water for diafiltration of the third-stage ultrafiltration membrane module was 0.5 t/h, and at the same time, a permeated solution of the third-stage diafiltration at a flow rate of 0.5 t/h was produced to be used as water for diafiltration of the second-stage, and a permeated solution of the second-stage diafiltration at a flow rate of 0.5 t/h was produced to be used as water for diafiltration of the first-stage.
When the system was stable, the sugar content in the residual solution of the third-stage diafiltration was approximately 2.19%, the sucrose content in the concentrated solution of the nanofiltration was approximately 11.32% with a colourity of 932 IU, and the recovery rate for residual sugar was 80.9%, the residual sugar loss accounted for 1.91% of the total sugar of the entire process, and the decolorization rate of the recovered concentrated solution of the nanofiltration was 93.4%.
The water consumption of a conventional dilution-concentration intermittent diafiltration (the diafiltration membrane module was a spiral polyether sulfone membrane module, with a molecular weight cut-off of 5000 Da, an operating temperature of 25 °C, a pressure of 0.5 MPa and a dilution multiple of 2) to obtain a
EX180270PPC-AU same residual sugar recovery rate was about 3.5 times that of the new process, the decolorization rate was reduced to 79.2%, and the sugar content in the decolourized solution of the diafiltration was only 3.2%.
By using the recovery device described in Example 1, water was saved by 71.4%, the decolorization rate was increased by 17.9%, and the sugar concentration in the recovered permeated solution of the diafiltration was increased by 254%.
The applicant states that the above descriptions are only specific embodiments of the present invention, the protection scope of the present invention is not limited thereto, and those skilled in the art should understand that any changes or substitutions which are easily obtained by those skilled belonged to the art within the technical scope disclosed by the present invention fall within the protection scope and disclosure scope of the present invention.

Claims (3)

    2016347128 01 Apr 2019 The claims defining the invention are as follows:
  1. (1) subjecting a sugar-containing solution to multi-stage countercurrent ultrafiltration to obtain a permeated solution of the first-stage ultrafiltration and a retentate of the last-stage ultrafiltration, and discharging the retentate of the last-stage ultrafiltration, the multi-stage countercurrent ultrafiltration is performed by 2-5 stages of ultrafiltration membrane modules, the ultrafiltration membrane module has a molecular weight cut-off of 1000-5000 Da, an operating temperature of 25-95 °C, and an operating pressure of 0.5-1.5 MPa;
    1. A device for recovering residual sugar in the membrane-based process of manufacturing sugar from sugarcane, comprising a multi-stage countercurrent diafiltration unit and a nanofiltration concentration unit, the multi-stage countercurrent diafiltration unit comprises at least 2 stages of ultrafiltration membrane modules, the nanofiltration concentration unit comprises a nanofiltration membrane module;
    the outlet on the retentate side of the previous-stage ultrafiltration membrane module of the multi-stage countercurrent diafiltration unit is connected to the inlet on the retentate side of the next-stage ultrafiltration membrane module, the inlet on the retentate side of the previous-stage ultrafiltration membrane module is connected to the outlet on the permeation side of the next-stage ultrafiltration membrane module;
    the outlet on the permeation side of the first-stage ultrafiltration membrane module of the multi-stage countercurrent diafiltration unit is connected to the inlet on the retentate side of the nanofiltration membrane module;
    a sugar-containing concentrated solution is obtained on the retentate side of the nanofiltration membrane module, and a pigment-containing retentate is obtained on the retentate side of the last-stage ultrafiltration membrane module of the multi-stage countercurrent diafiltration unit;
    the outlet on the permeation side of the nanofiltration membrane module is connected to the inlet on the retentate side of the last-stage nanofiltration membrane module of the multi-stage countercurrent diafiltration unit.
  2. (2) subjecting the permeated solution of the first-stage ultrafiltration to nanofiltration concentration to obtain a sugar-containing concentrated solution and a permeated solution of the nanofiltration, the nanofiltration concentration is performed by a nanofiltration membrane module, the nanofiltration membrane module has a membrane molecular weight cut-off of 90-400 Da, an operating temperature of 25-95 °C and an operating pressure of 2.0-4.1 MPa;
    2:3-1:5.
    10. The method according to any one of claims 5 to 9, characterized in that the method comprises the following steps:
    (2) subjecting the permeated solution of the first-stage ultrafiltration to nanofiltration concentration to obtain a sugar-containing concentrated solution and a permeated solution of the nanofiltration; and the permeated solution of the nanofiltration is used as water for diafiltration for the multi-stage countercurrent ultrafiltration in step (1).
    6. The method according to claim 5, characterized in that the sugar-containing solution in step (1) is a concentrated solution of mixed sugarcane juice, which has been concentrated 10-30 times by microfiltration pretreatment and ultrafiltration decoloration treatment;
    preferably, the manner of the multi-stage countercurrent ultrafiltration in step (1) is equal-volume countercurrent ultrafiltration;
    preferably, the water used for diafiltration in the multi-stage countercurrent ultrafiltration in step (1) is deionized water;
    preferably, the volume of the water used for diafiltration in step (1) is 1-3 times of the volume of the sugar-containing solution;
    Preferably, the retentate of the last-stage ultrafiltration in step (1) is used to extract natural pigments.
    7. The method according to claim 5 or 6, characterized in that the multi-stage countercurrent ultrafiltration in step (1) is performed by 2-5 stages of ultrafiltration membrane modules;
    preferably, the ultrafiltration membrane module has a molecular weight cut-off of 1000-5000 Da;
    EX180270PPC-AU
    2016347128 01 Apr 2019 preferably, the ultrafiltration membrane module has an operating temperature of 25-95 °C;
    preferably, the ultrafiltration membrane module has an operating pressure of 0.5-1.5 MPa;
    preferably, the ultrafiltration membrane module is in a spiral, tubular, flat, or hollow fiber form;
    preferably, the material of the ultrafiltration membrane module is polysulfone, polyether sulfone, sulfonated polyether sulfone or polyvinylidene fluoride.
    8. The method according to any one of claims 5 to 7, characterized in that the nanofiltration concentration of step (2) is performed by a nanofiltration membrane module;
    preferably, the nanofiltration membrane module has a membrane molecular weight cut-off of 90-400 Da, preferably 200 Da;
    preferably, the nanofiltration membrane module has an operating temperature of 25-95 °C;
    preferably, the nano filtration membrane module has an operating pressure of 2.0-4.1 MPa;
    preferably, the nanofiltration membrane module is in the form of spiral membrane;
    preferably, the sugar-containing concentrated solution of step (2) is crystallized by evaporation to obtain sugar.
    9. The method according to any one of claims 5 to 8, characterized in that the volume ratio of the permeated solution of the nanofiltration in step (2) to the water for diafiltration for the multi-stage countercurrent ultrafiltration in step (1) is between
    EX180270PPC-AU
    2016347128 01 Apr 2019
    2. The device according to claim 1, characterized in that the diafiltration manner of the multi-stage countercurrent diafiltration unit is equal-volume countercurrent diafiltration.
    EX180270PPC-AU
    2016347128 01 Apr 2019
    3. The device according to claim 1 or 2, characterized in that the multi-stage countercurrent diafiltration unit comprises 2-5 stages of ultrafiltration membrane modules;
    preferably, the ultrafiltration membrane module has a molecular weight cut-off of 1000-5000 Da;
    preferably, the ultrafiltration membrane module has an operating temperature of 25-95 °C;
    preferably, the ultrafiltration membrane module has an operating pressure of 0.5-1.5 MPa;
    preferably, the ultrafiltration membrane module is in a spiral, tubular, flat, or hollow fiber form;
    preferably, the material of the ultrafiltration membrane module is polysulfone, polyether sulfone, sulfonated polyether sulfone or polyvinylidene fluoride.
    4. The device according to any one of claims 1 to 3, characterized in that the nanofiltration membrane module is in the form of spiral membrane;
    preferably, the nanofiltration membrane module has a membrane molecular weight cut-off of 90-400 Da, preferably 200 Da;
    preferably, the nanofiltration membrane module has an operating temperature of 25-95 °C;
    preferably, the nano filtration membrane module has an operating pressure of 2.0-4.1 MPa.
    5. A method for recovering residual sugar by using the device according to any one of claims 1 to 4, comprising the following steps:
    EX180270PPC-AU
    2016347128 01 Apr 2019 (1) subjecting a sugar-containing solution to multi-stage countercurrent ultrafiltration to obtain a permeated solution of the first-stage ultrafiltration and a retentate of the last-stage ultrafiltration, and discharging the retentate of the last-stage ultrafiltration;
  3. (3) using the permeated solution of the nanofiltration and the deionized water in a volume ratio of 2:1-1:4 as water for diafiltration for the multi-stage countercurrent ultrafiltration in step (1).
AU2016347128A 2015-10-28 2016-10-26 Apparatus and method for recovering residual sugar in cane sugar manufacturing process Active AU2016347128B2 (en)

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