CN110904280A - Method for decoloring sugar juice by using water-soluble zinc salt-lime - Google Patents
Method for decoloring sugar juice by using water-soluble zinc salt-lime Download PDFInfo
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- 239000000049 pigment Substances 0.000 abstract description 15
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 abstract description 14
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Classifications
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/005—Purification of sugar juices using chemicals not provided for in groups C13B20/02 - C13B20/14
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Non-Alcoholic Beverages (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to a method for decoloring sugar juice by using water-soluble zinc salt-lime, which comprises the following specific steps: adding water soluble zinc salt into sugar juice, adjusting pH with lime milk, stirring at 65-80 deg.C for 10-30min, adding PAM, standing for separation, and standing to obtain clear juice after flocculation and settling are stable. The method takes zinc sulfate (zinc sulfate, zinc chloride or zinc nitrate) as an inorganic decolorizing agent, generates zinc hydroxide and calcium salt (calcium sulfate, calcium oxide or calcium nitrate) by coagulation reaction under an alkaline condition, adsorbs or embeds non-sugar substances such as pigments and the like in sugar juice, has the decolorizing rate of 81.75 percent, has simple process, does not adopt toxic and harmful substances, and belongs to a green clarification decolorizing process. The principle is as follows: the zinc salt is used as an inorganic decolorant, and is subjected to coagulation reaction under an alkaline condition to generate zinc hydroxide and calcium salt, and non-sugar substances such as pigments in the sugar juice are adsorbed or embedded.
Description
Technical Field
The invention relates to a method for decoloring sugar juice by using water-soluble zinc salt-lime, belonging to the field of sugar juice clarification and decoloring.
Background
The pigment molecules of sugar juice can be divided into two main categories: fat-soluble pigments and water-soluble pigments. The fat-soluble pigment is insoluble in water, mainly contains chlorophyll, lutein, carotene and the like, is usually mixed with various cane fats in cane juice, is covered and protected by protein, and is dispersed into suspended particles; the water-soluble pigment is mainly various phenolic substances, and the variety of the phenolic substances is various and complicated, and the phenolic substances are often changed into darker substances in the production process, so that the water-soluble pigment has great adverse effect on the sugar making process. At present, clarification and decoloration processes in the sugar industry mainly comprise a phosphoric acid-lime method, a sulfurous acid method, a carbonic acid method, an activated carbon adsorption method, a hydrogen peroxide oxidation method and the like, but have the defects of poor clarification and decoloration effects, environmental pollution, high cost, complex oxidation products and the like. Therefore, the need for decolorization and impurity removal of sugar juice has become a hot point of research in the sugar industry in recent years, and is also a difficulty.
Enemy, the Sanjun researches the decolorization of the calcium sulfate on the dye wastewater, the decolorization effect is obvious, and nitrogen and phosphorus compounds in the water body can be removed while the decolorization is carried out. Calcium sulfate is added into the process for treating wastewater in the poplar and the shuangchun, and the like, so that the decoloring effect is further enhanced. The Qiu's sword and the like research the optimal adsorption conditions of the calcium sulfate on impurities and phosphorus in the wastewater, and the results show that the adsorption effect of the calcium sulfate under the alkaline condition is more remarkable than that under the acidic condition. Zinc hydroxide is a typical amphoteric hydroxide and is widely used as an antibacterial agent, a filler, a neutralizer, a catalyst, and the like. At present, few studies on the decolorization of sugar juice by nascent zinc hydroxide are reported.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method uses zinc salt (zinc sulfate, zinc chloride or zinc nitrate) as inorganic decolorant, and produces zinc hydroxide and calcium salt (calcium sulfate, calcium oxide or calcium nitrate) by coagulation reaction under alkaline condition, and adsorbs or embeds non-sugar substances such as pigment in sugar juice, and the decoloration rate reaches 81.75%.
The technical scheme for solving the technical problems is as follows: a method for decoloring sugar juice with water-soluble zinc salt-lime comprises adding water-soluble zinc salt into sugar juice to make zinc ion content at 1000mg/L of 300-.
The water-soluble zinc salt is zinc sulfate, zinc chloride or zinc nitrate.
The sugar juice is sugarcane mixed juice or brown granulated sugar or raw sugar redissolved syrup
The invention provides a water-soluble zinc salt-lime method, for example, the method adopts zinc sulfate and lime cream to react in sugar juice to obtain calcium sulfate and zinc hydroxide, the calcium sulfate can be used as a decoloring agent for clarifying and decoloring the sugar juice, the decoloring rate is high, the process is simple, the cost is low, toxic and harmful substances are not adopted, the method belongs to a green clarifying and decoloring process, and the method has a certain application prospect in the sugar industry. The principle is as follows: zinc salt (zinc sulfate, zinc chloride or zinc nitrate) is used as an inorganic decolorizing agent, zinc hydroxide and calcium salt (calcium sulfate, calcium oxide or calcium nitrate) are generated through coagulation reaction under an alkaline condition, and under the optimal process condition, namely the zinc salt dosage is 800mg/L, the system pH is 8.0, the system temperature is 75 ℃, the reaction time is 10min, and the sugar juice decolorizing rate is as high as 81.75% (proved by experiments, the process condition can also achieve the same effect in practical production application).
The technical characteristics of the method for decoloring sugar juice by using water-soluble zinc salt-lime of the invention are further explained by combining the attached drawings and the embodiment.
Drawings
FIG. 1: the influence curve of the zinc salt dosage on the decolorization rate of the brown granulated sugar redissolution syrup.
FIG. 2: the influence curve of the system pH value on the decolorization rate of the brown granulated sugar redissolved syrup.
FIG. 3: the influence of time on the decolorization rate of brown granulated sugar redissolved syrup is shown in a graph.
FIG. 4: the influence curve of the system temperature on the decolorization rate of the brown granulated sugar redissolved syrup.
FIG. 5: zeta potential diagram of the system under different conditions. Wherein a, b and c represent Zeta potentials of blank systems with pH values of 7, 8 and 9; d represents Zeta potential of the sugar juice after the treatment under the optimal condition; e represents the Zeta potential of the untreated sugar juice. As can be seen from fig. 5, the Zeta potential of the blank system gradually decreases from large to small in absolute value with the increase of pH, and is positive, which indicates that the surface of the colloidal particles in the blank solution is positively charged. The Zeta potential of the sugar juice treated under the optimal conditions is measured to be-4.13 mV, the Zeta potential of the original sugar juice is measured to be-10.16 mV, and the potential of the colloidal particles of the blank system is measured to be 5.83 mV when the pH value is 8, because the nascent colloidal particles neutralize the colloidal particles and the non-sugar components with negative electricity in the sugar juice through adsorption, so that the Zeta potential of the system is converted from a positive value to a negative value, and the decolorization mechanism can be preliminarily judged to have the electric neutralization adsorption.
FIG. 6: SEM image of the precipitate before adsorption. FIG. 6 is an SEM image of the formation of a precipitate in a blank solution, flower-like, loose surface.
FIG. 7: SEM images of the precipitate after adsorption in sugar juice. FIG. 7 is an SEM image after reaction in sugar juice, flaked but with a dense surface. Because the precipitate adsorbs pigment molecules of the sugar juice, the Zeta potential on the surface of the particles is reduced, so that the aggregation among colloidal particles is caused, and finally, large and compact precipitate is generated.
FIG. 8: infrared spectra before and after adsorption. As can be seen from FIG. 8, the IR spectra of the precipitates before and after adsorption were changed to 2927.3 cm after adsorption-1Around the peak, a new peak appears, probably from-CH2Due to elastic vibration of C-H in the radical; after adsorption, the concentration is 1043 cm-1New peaks appear on the left and right, and the peaks may be C-O stretching vibration peaks of phenolic substances; the red shift or blue shift of some absorption peak positions is compared before and after, and the precipitate is acted on the non-sugar components, so that the initial judgment of the aggregate on the non-sugar components and the like can be madeThe substance has adsorption effect.
Detailed Description
Example 1: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc sulfate to ensure that the content of zinc ions is 800mg/L, then adjusting the pH value to 8.0 by lime milk, keeping stirring at the temperature of 75 ℃ for 10min, adding 2mg/L PAM, standing and separating, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the pore diameter of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 81.75%.
Example 2: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc sulfate to ensure that the content of zinc ions is 750mg/L, then adjusting the pH value to 8.5 by lime milk, keeping stirring at 65 ℃ for 10min, adding 2mg/L PAM, standing and separating, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the aperture of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 80.39%.
Example 3: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc sulfate to ensure that the content of zinc ions is 750mg/L, then adjusting the pH value to 8.0 by lime milk, keeping stirring at the temperature of 70 ℃ for 10min, adding 2mg/L PAM, standing and separating, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the aperture of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 80.47%.
Example 4: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc sulfate to ensure that the content of zinc ions is 750mg/L, then adjusting the pH value to 7.5 by lime milk, keeping stirring at 65 ℃ for 10min, adding 2mg/L PAM, standing and separating, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the aperture of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 80.30%.
Example 5: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc sulfate to ensure that the content of zinc ions is 800mg/L, then adjusting the pH value to 8.0 by lime milk, keeping stirring at 65 ℃ for 10min, adding 2mg/L PAM, standing and separating, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the aperture of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 81.74%.
Example 6: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc nitrate to ensure that the content of zinc ions is 750mg/L, then adjusting the pH value to 8.0 by lime milk, keeping stirring at the temperature of 70 ℃ for 10min, adding 2mg/L PAM, standing for separation, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the pore diameter of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 80.30%.
Example 7: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc chloride to ensure that the content of zinc ions is 700mg/L, then adjusting the pH value to 8.0 by lime milk, keeping stirring at the temperature of 75 ℃ for 10min, adding 2mg/L PAM, standing and separating, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the pore diameter of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 80.16%.
Example 8: taking 100 mL brown granulated sugar redissolved syrup with 10 degrees of Bx, putting the syrup into a 250mL beaker, adding zinc nitrate to ensure that the content of zinc ions is 800mg/L, then adjusting the pH value to 7.5 by lime milk, keeping stirring at the temperature of 70 ℃ for 10min, adding 2mg/L PAM, standing for separation, obtaining clean juice after flocculation and sedimentation are stable, taking a certain volume of supernatant to adjust the pH value to 7.00 +/-0.02, then filtering by using an organic filter membrane with the pore diameter of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate to be 81.21%.
The invention adopts the following method to calculate the decolorization ratio:
the color value measurement was carried out in accordance with the regulations of International organization ICUMSA (International Committee for the unified methods for sugar analysis). Adjusting the pH value of the sugar solution to 7.00, filtering, collecting filtrate, and measuring the absorbance, the refractive index and the solution temperature of the filtrate at the wavelength of 560 nm. Thereby calculating the color value of the sugar solution.
The calculation formula is as follows:
wherein:IU 560-a color value;A 560-absorbance measured at a wavelength of 560 nm;b-thickness of cuvette (cm);
cthe concentration of solute in the sample solution (g/mL) can be calculated by the following formula: c = refractive brix of the juice x corresponding apparent density (20 ℃)/100.
The decolorization ratio is calculated by the following formula:
wherein: d-decolorization (%); IU (International Union of China)Front side-sugar liquor colour value before treatment; IU (International Union of China)Rear end-color value of processed sugar solution.
Single factor experiment of the present invention
The experimental method comprises the following steps: taking 100 mL of 10-degree Bx brown granulated sugar redissolved syrup, putting the syrup into a 250mL beaker, adding a certain amount of zinc sulfate solution, adjusting the pH value, reacting at a certain temperature for a period of time, adding 2mg/L PAM, standing, separating, taking a certain volume of supernatant until the pH value is adjusted to 7.00 +/-0.02, filtering by using an organic filter membrane with the aperture of 0.45 mu m, measuring the absorbance at 560 nm, and calculating the decolorization rate.
1. Effect of Zinc salt amount on decoloring ratio
Controlling the temperature of the system at 30 ℃, adding a certain amount of zinc salt (0, 250, 500, 750 and 1000 mg/L), adjusting the pH to 7.00 by using lime milk, reacting for 30min, adding PAM, standing for separation, measuring the absorbance of the mixture under a certain condition, and calculating related parameters. The effect of zinc salt dosage on decolorization rate was examined and the results are shown in FIG. 1. With the increase of the zinc salt dosage, the decolorization rate is obviously improved. The pigment molecules of the juice are adsorbed due to the formation of nascent calcium salts (calcium sulfate, calcium oxide or calcium nitrate) and zinc hydroxide. When the zinc salt is used in an amount of 750 mg.L-1When the above time points, the decolorization rate tends to be highThe potential is mild, mainly because the adsorption reaches a saturated state when the generated adsorbent reaches a certain value, and the adsorption reaches equilibrium.
2. Effect of System pH on decolorization Rate
Controlling the temperature of the system at 30 ℃, adding 750mg/L zinc salt, adjusting the pH to 5.0, 6.0, 7.0, 8.0 and 9.0 respectively by using lime milk, reacting for 30min, adding PAM, standing, separating, measuring the absorbance under certain conditions, and calculating related parameters. The effect of pH on destaining was examined and the results are shown in FIG. 2. When the pH value of the system is between 5.0 and 8.0, the decolorization rate is increased along with the increase of the pH value; when the pH exceeded 8.0, the decolorization rate began to drop. Therefore, the optimum system pH is selected to be 8.0. On one hand, the pH value of the system is increased, and the amount of newly generated zinc hydroxide is increased, so that more pigment molecules can be adsorbed; on the other hand, pH affects the charge density of nascent calcium salts (calcium sulfate, calcium oxide or calcium nitrate), nascent zinc hydroxide surfaces, and thus the amount of electrically neutralized adsorbed pigment molecules.
3. Effect of reaction time on decolorization ratio
Controlling the temperature of the system at 30 ℃, adding 750mg/L zinc salt, adjusting the pH value to 8.0 by lime milk, changing the reaction time (10 min, 20 min, 30min, 40 min and 50 min) of the system, adding PAM, standing for separation, measuring the absorbance of the PAM under certain conditions, and calculating related parameters. The effect of pH on destaining was examined and the results are shown in FIG. 3. The reaction time has minimal effect on the decolorization ratio as can be seen by range analysis. Within 10-50 min, the decolorization rate is only changed by about 3%, which shows that the pigment molecules in the sugar juice are adsorbed by the nascent calcium salt (calcium sulfate, calcium oxide or calcium nitrate) and the nascent zinc hydroxide by non-sugar components, and the process is a rapid process. The reaction time was selected to be 10min, taking into account the time cost of the process.
4. Effect of System temperature on decolorization Rate
Changing the temperature of the system (30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃ and 90 ℃), adding 750mg/L zinc salt, controlling the pH of the system to be 8.0, reacting for 10min, adding PAM, standing for separation, measuring the absorbance of the solution under certain conditions, and calculating related parameters. The effect of temperature on decolorization was examined and the results are shown in FIG. 4. The decoloring rate changes remarkably at 30-60 ℃; after a temperature of 60 ℃ the discoloration changes slowly. The brownian motion of various particles in the sugar juice is accelerated by raising the temperature, and simultaneously, the viscosity of the sugar juice is reduced, so that the effective collision of pigment molecules with the new calcium salt (calcium sulfate, calcium oxide or calcium nitrate) and the new zinc hydroxide is increased, and the decolorization rate is improved. The adsorption rate is close to the resolution rate and the decolorization rate is almost unchanged due to the overhigh temperature.
Claims (3)
1. A method for decoloring sugar juice by using water-soluble zinc salt-lime is characterized by comprising the following steps: adding water soluble zinc salt into the sugar juice to ensure that the content of zinc ions is 1000mg/L at 300-80 ℃, adjusting the pH value to 7-9 by lime milk, continuously stirring for 10-30min at the temperature of 65-80 ℃, then adding 1-5mg/L PAM into the sugar juice, standing for separation, and obtaining clean juice after flocculation and sedimentation are stable.
2. The method for decoloring sugar juice according to claim 1, wherein the water-soluble zinc salt-lime is selected from the group consisting of: the water-soluble zinc salt is zinc sulfate, zinc chloride or zinc nitrate.
3. The process according to claim 1 or 2 for sugar juice decolouration of water soluble zinc salt-lime, characterized in that: the sugar juice is sugarcane mixed juice or brown granulated sugar or raw sugar redissolution syrup.
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| CN113881816A (en) * | 2020-07-01 | 2022-01-04 | 广西科技大学 | Sugarcane juice cleaning method |
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