CN114471168A - Method for separating and concentrating beet polysaccharide and betaine by combining thermal flocculation with multi-stage nanofiltration membrane - Google Patents
Method for separating and concentrating beet polysaccharide and betaine by combining thermal flocculation with multi-stage nanofiltration membrane Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 88
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 59
- 235000016068 Berberis vulgaris Nutrition 0.000 title claims abstract description 42
- 241000335053 Beta vulgaris Species 0.000 title claims abstract description 42
- 150000004676 glycans Chemical class 0.000 title claims abstract description 41
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 41
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 41
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 title claims abstract description 38
- 229960003237 betaine Drugs 0.000 title claims abstract description 38
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004062 sedimentation Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 16
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000012466 permeate Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 9
- 235000015191 beet juice Nutrition 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
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- 238000002386 leaching Methods 0.000 claims description 4
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- 239000000203 mixture Substances 0.000 claims 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/10—Temperature control
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/14—Pressure control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/18—Details relating to membrane separation process operations and control pH control
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/22—Details relating to membrane separation process operations and control characterised by a specific duration or time
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2626—Absorption or adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2642—Aggregation, sedimentation, flocculation, precipitation or coagulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2673—Evaporation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
Abstract
The invention discloses a method for separating and concentrating beet polysaccharide and betaine by combining thermal flocculation with a multi-stage nanofiltration membrane. Belongs to the technical field of effective component separation. The method comprises the following steps: pre-treating; thermal flocculation; clarifying and decoloring; a continuous nanofiltration membrane process; concentrating polysaccharide; and (4) concentrating the betaine. According to the invention, the beet exudate is subjected to flocculation clarification by adopting the composite high-temperature flocculant, so that the sedimentation performance of complex organic suspended matters in the exudate is greatly improved, the content of suspended substances such as pectin and the like is reduced, and the viscosity of feed liquid is reduced, so that the pressure of membrane operation is reduced, membrane work can be stably carried out for a long time, and the service life of a nanofiltration membrane is prolonged; the activated carbon is used for adsorbing the pigment, so that the yield of the beet polysaccharide and the betaine is increased. The method has the characteristics of high efficiency, environmental protection, low cost and high yield, is a method for continuously recovering effective active ingredients with different molecular weights from the beet extract, can be applied to a sugar manufacturing process, and helps to reduce the discharge of waste honey and other wastes.
Description
Technical Field
The invention relates to the technical field of effective component separation, in particular to a method for separating and concentrating beet polysaccharide and betaine by using thermal flocculation combined with a multi-stage nanofiltration membrane.
Background
Beet is one of the main sugar crops in China, and the sugar production of beet accounts for about 25 percent of the global sugar production, and the production scale and the generated economic benefit are huge. In order to improve the purity of sugar products, most of domestic sugar factories adopt a carbonation cleaning process to clarify beet exudation juice in the sugar production process by a double carbonic acid method, but the process has high energy consumption and low sugar production efficiency, and a large amount of non-sugar components are still remained in concentrated sugar liquid and are not effectively removed, thereby influencing the crystallization rate and the quality of the final sugar products. The non-sugar active components comprise pigment substances, organic macromolecular substances (polysaccharide and pectin) and micromolecular substances (betaine and reducing sugar), and the non-sugar active components become waste honey and then flow into underground water through discharge, so that serious water pollution and resource waste are caused.
The beet polysaccharide is an active polysaccharide with a molecular weight range of 0.74-300 kDa, and has important physiological activities of oxidation resistance, bacteriostasis, immune function regulation and the like. Betaine is a quaternary ammonium type alkaloid, has a molecular weight of 117.15, has activities of resisting oxidation, improving cardiovascular diseases, improving intestinal functions, resisting tumors and the like, and is widely applied to the fields of clinical treatment, foods, cosmetics and the like.
However, the current beet sugar-making process can not process the beet polysaccharide and the betaine and can not reasonably and fully recover and develop the value of the beet polysaccharide and the betaine.
Therefore, how to provide a method for separating and concentrating beet polysaccharide and betaine is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for separating and concentrating beet polysaccharide and betaine by using thermal flocculation combined with a multi-stage nanofiltration membrane. The beet leachate is treated by combining a thermal flocculation method with a multi-stage nanofiltration membrane, so that the content of suspended matters (including pectin) in the beet leachate is reduced, the stability of the membrane capable of working for a long time is ensured, the yield of beet polysaccharide and betaine is improved, and the requirements of sugar making processes are met
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for separating and concentrating beet polysaccharide and betaine by using thermal flocculation combined with a multi-stage nanofiltration membrane comprises the following steps:
s1, pretreatment: using water as an extracting solution for beet, and carrying out exudation and impurity removal to obtain a beet juice leaching solution;
s2, thermal flocculation: mixing the beet juice leachate obtained in the step S1 with a composite high-temperature flocculant, heating to obtain floccules, and performing inclined plate sedimentation to obtain a supernatant;
s3, clarifying and decoloring: clarifying the supernatant in the S2 by an ultrafiltration membrane and decoloring by active carbon to obtain feed liquid;
s4, continuous nanofiltration membrane process: placing the feed liquid in a continuous nanofiltration membrane device, and performing primary nanofiltration to obtain trapped fluid 1 and permeate fluid 1, wherein the trapped fluid 1 is polysaccharide concentrated solution; the permeate 1 enters secondary nanofiltration to obtain trapped fluid 2 and permeate 2, the permeate 2 is a betaine concentrated solution, and the trapped fluid 2 is a sucrose concentrated solution;
s5, polysaccharide concentration: concentrating the trapped fluid 1, and freeze-drying;
s6 betaine concentration: the permeate 2 was concentrated and freeze-dried.
Further, cleaning and shredding beet, and extracting;
oozing using oozing devices;
removing impurities with a cyclone.
Preferably: step S2 compounding ingredients of the high temperature flocculant: the mass ratio of polyacrylamide to polysilicic acid is 1: 1, mixing; the addition amount of the composite high-temperature flocculant is 3-5 ppm.
Preferably: step S2, heating to 80-85 ℃ for 15-20 min; the time of inclined plate sedimentation is 20-30 min.
Preferably: the inclined plate sedimentation in step S2 at least satisfies 300m3Water inflow of/h and 270m3Water yield per hour.
Further, inclined plate clarifiers are used for inclined plate sedimentation.
Preferably: in the step S3, the aperture of the ultrafiltration membrane is 15-20 kDa, and the pressure behind the membrane is controlled to be 0.2-0.3 Mpa; decoloring by using activated carbon, controlling the pH to be 9-10 stably, controlling the temperature to be 45-55 ℃, and controlling the time to be 15-20 min.
Further, activated carbon is decolorized by using a decolorizing tank.
Preferably: the molecular weight cut-off of the primary nanofiltration membrane in the step S4 is 200-800 Da; the molecular weight cut-off of the secondary nanofiltration membrane is more than or equal to 150Da and less than 200 Da; the pressure range before the membrane of the continuous nanofiltration membrane device is controlled to be 1.0-8.0 MPa, the temperature is controlled to be 35-55 ℃, the pH value in the primary nanofiltration process and the secondary nanofiltration process is controlled to be 9-10, and the time is controlled to be 60-90 min.
Preferably: in the step S4, the pressure before the membrane of the continuous nanofiltration membrane device is 3.0MPa, and the temperature is 55 ℃.
Preferably: in the step S5, the concentration temperature is 75-80 ℃, and the vacuum degree is 0.1-0.2 MPa.
Preferably: in the step S6, the concentration temperature is 70-80 ℃, and the vacuum degree is 0.1-0.2 MPa.
According to the technical scheme, compared with the prior art, the invention discloses and provides the method for separating and concentrating the beet polysaccharide and the betaine by using the thermal flocculation combined with the multi-stage nanofiltration membrane, and the obtained technical effects are that the beet exudate is subjected to flocculation clarification by using the composite high-temperature flocculant, so that the sedimentation performance of complex organic suspended matters in the exudate is greatly improved, the content of suspended matters such as pectin and the like is reduced, the viscosity of feed liquid is reduced, the pressure of membrane operation is reduced, membrane work can be stably carried out for a long time, and the service life of the nanofiltration membrane is prolonged; the activated carbon is used for adsorbing the pigment, so that the yield of the beet polysaccharide and the betaine is increased. The method has the characteristics of high efficiency, environmental protection, low cost and high yield, is a method for continuously recovering effective active ingredients with different molecular weights from the beet extract, can be applied to a sugar manufacturing process, and helps to reduce the discharge of waste honey and other wastes.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a flow chart of a separation and concentration process provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a method for separating and concentrating beet polysaccharide and betaine by using thermal flocculation combined with a multi-stage nanofiltration membrane.
The raw materials and equipment which are not described in detail in the examples are all commercially available conventional production testing equipment, and are not described herein again.
Example 1
A method for separating and concentrating beet polysaccharide and betaine by using thermal flocculation combined with a multi-stage nanofiltration membrane comprises the following steps:
s1, pretreatment: cleaning and shredding beet, percolating with water in a percolating device, and removing impurities in a cyclone to obtain beet juice leachate;
s2 thermal flocculation: mixing the beet juice leachate with a composite high-temperature flocculating agent (mixing polyacrylamide and polysilicic acid according to a mass ratio of 1: 1), adjusting the heating temperature to 80 ℃, keeping the heating temperature for 15min, and measuring the addition of the composite high-temperature flocculating agent to be 3ppm, so as to obtain floccule, and measuring the sediment amount in 10min, 20min and 30min respectively, namely the volume of the bottom suspended matter after full sedimentation; after full sedimentation, measuring the volume ratio of the supernatant to the sediment, wherein the volume ratio is respectively 2mL/50mL, 4mL/50mL and 7mL/50mL, the sedimentation effect is obvious in 30min, and the removal effect is obvious for non-target products;
s3, clarifying and decoloring: clarifying the supernatant in the S2 by an ultrafiltration membrane and decoloring by active carbon to obtain feed liquid;
s4, continuous nanofiltration membrane process: the feed liquid is placed in a continuous nanofiltration membrane device and subjected to primary nanofiltration to obtain trapped fluid 1 which is polysaccharide concentrated solution, the permeate liquid 1 enters secondary nanofiltration to obtain permeate liquid 2 which is betaine concentrated solution, and the trapped fluid 2 is sucrose concentrated solution;
s5, polysaccharide concentration: concentrating the trapped fluid 1, and freeze-drying to obtain a dried beet polysaccharide product III;
s6 betaine concentration: concentrating the permeate 2, and freeze-drying to obtain a betaine crude dry product III;
in order to further optimize the technical scheme:
the inclined plate sedimentation process in S2 is completed in an inclined plate clarifier and at least meets 300m3Water inflow and 270m3Water yield per hour;
s3, the ultrafiltration membrane is a tubular ultrafiltration membrane, the aperture is 15kDa, and the pressure behind the membrane is controlled at 0.3 Mpa; decolorizing with activated carbon in a decolorizing tank, controlling pH to be 9.0, temperature to be 50 deg.C, and time to be 15 min;
the types of the multi-stage nanofiltration membranes in the S4 are roll-type ultrafiltration membranes (the molecular weight cut-off of a first-stage nanofiltration membrane is 200Da, the molecular weight cut-off of a second-stage nanofiltration membrane is 150Da, the pressure range of the continuous nanofiltration membrane device is controlled to be 1.0MPa, the temperature is controlled to be 35 ℃, the pH value in the processes of the first-stage nanofiltration and the second-stage nanofiltration is controlled to be 9, and the time is 60 min);
in the S5, the concentration temperature is 80 ℃, and the vacuum degree is 0.1 MPa;
in S6, the concentration temperature is 70 ℃, and the vacuum degree is 0.1 MPa.
Example 2
The only difference from example 1 is the following process parameter adjustment:
the addition amount of the composite high-temperature flocculant in S2 is 4 ppm;
heating to 85 deg.C for 15 min;
the inclined plate clarifier is used for inclined plate sedimentation and at least meets 300m3Water inflow and 270m3Water yield per hour;
in S2, sediment amount is measured respectively at 10min, 20min and 30min, volume ratio of supernatant to sediment is measured after full sedimentation, the volume ratio is respectively 2mL/50mL, 5.5mL/50mL and 8mL/50mL, sedimentation effect is obvious at 30min, and effect of removing non-target products is obvious;
the aperture of the ultrafiltration membrane in the S3 is 20kDa, and the pressure behind the membrane is controlled at 0.2 Mpa; decolorizing with activated carbon in a decolorizing tank, controlling pH to be 9.5, temperature to be 50 deg.C, and time to be 15 min;
the molecular weight cut-off of the primary nanofiltration membrane in the step S4 is 500 Da; the molecular weight cut-off of the secondary nanofiltration membrane is 150 Da; the temperature is 45 ℃, the pressure range before the membrane of the continuous nanofiltration membrane device is controlled to be 5.0MPa, the pH value in the primary nanofiltration process and the secondary nanofiltration process is controlled to be 9.5, and the time is 60 min;
and concentrating and drying the trapped fluid 1 and the permeate liquid 2 to obtain a crude dried product IV of the beet polysaccharide and a crude dried product IV of the betaine.
Example 3
The difference from example 1 is in the process parameter adjustment:
the addition amount of the composite high-temperature flocculant in S2 is 5 ppm;
heating to 85 deg.C for 15 min;
the inclined plate clarifier is used for inclined plate sedimentation and at least meets 300m3Water inflow of/h and 270m3Water yield per hour;
in S2, sediment amount is measured respectively at 10min, 20min and 30min, volume ratio of supernatant to sediment is measured after full sedimentation, the volume ratio is respectively 3mL/50mL, 9mL/50mL and 10mL/50mL, sedimentation effect is obvious at 20min, and effect of removing non-target products is obvious;
s3, the aperture of the ultrafiltration membrane is 15kDa, the pressure behind the membrane is controlled at 0.3Mpa, the activated carbon decoloration is carried out by using a decoloration tank, the pH is controlled to be stable at 10, the temperature is controlled to be stable at 50 ℃, and the time is controlled to be 15 min;
the molecular weight cut-off of the primary nanofiltration membrane in the step S4 is 800 Da; the molecular weight cut-off of the secondary nanofiltration membrane is 150 Da; the temperature is 55 ℃, the pressure range before the membrane of the continuous nanofiltration membrane device is controlled to be 3.0MPa, the pH value in the primary nanofiltration process and the secondary nanofiltration process is controlled to be 10, and the time is 60 min;
concentrating and drying the trapped fluid 1 and the permeate liquid 2 to obtain a crude dried product V of the beet polysaccharide and a crude dried product V of the betaine.
Comparative experiment
1. Experiment of flocculation treatment leaching liquid of single flocculant and composite flocculant
S1, pretreatment: cleaning and shredding beet, percolating with water in a percolating device, and removing impurities in a cyclone to obtain beet juice leachate;
s2 thermal flocculation: mixing the beet leaching solution with polyacrylamide, polysilicic acid and a composite flocculant: the mass ratio of polyacrylamide: polysilicic acid is 1: 1, adjusting the heating temperature to 85 ℃, keeping the heating temperature for 15min, and adding 3ppm of high-temperature flocculating agent. Then, the feed liquid can complete the sedimentation within 30 min;
the viscosity of the leachate before and after flocculation in step S2 was measured using a viscometer as shown in table 1:
TABLE 1 feed liquid viscosity change after flocculation treatment of different flocculants
According to the table, the composite flocculant is preferably selected, and the leachate treated by the composite flocculant is collected to be subjected to the following steps:
s3, clarifying and decoloring: clarifying the supernatant in S2 with ultrafiltration membrane (the pore diameter of the ultrafiltration membrane is 15kDa, and the pressure after the membrane is controlled at 0.2Mpa) and decolorizing with active carbon to obtain feed liquid (pH is controlled at 9.5, temperature is controlled at 50 deg.C, and time is controlled at 15 min);
s4, concentrating and drying: concentrating and drying the clarified and decolored feed liquid to obtain a crude and dried product I of the beet polysaccharide betaine;
the type of the ultrafiltration membrane in the S3 is a tubular ultrafiltration membrane, the aperture is 20kDa, and the membrane back pressure is kept at 0.2 Mpa;
the concentration temperature in the S4 is 80 ℃, and the vacuum degree is 0.1 MPa.
2. Experiment for treating leachate by using continuous nanofiltration membrane
S1, pretreatment: cleaning and shredding beet, percolating with water in a percolating device, and removing impurities in a cyclone to obtain beet juice leachate;
s2, clarifying and decoloring: clarifying the percolate in the S1 by an ultrafiltration membrane and decoloring by active carbon;
s3, a continuous nanofiltration membrane process: subjecting the clarified and decolorized feed liquid to primary nanofiltration to obtain trapped fluid 1 which is polysaccharide concentrated solution, subjecting the permeated fluid 1 to secondary nanofiltration to obtain permeated fluid 2 which is betaine concentrated solution, and subjecting the trapped fluid 2 to sucrose concentrated solution;
s4, polysaccharide concentration: concentrating the trapped fluid 1, and freeze-drying to obtain a dried beet polysaccharide product II;
s5 betaine concentration: concentrating the permeate 2, and freeze-drying to obtain a betaine crude dry product II;
wherein the ultrafiltration membrane in the S2 is a tubular ultrafiltration membrane with a pore diameter of 20kDa, and the pressure after the membrane is kept at 0.2 Mpa;
the types of the multi-stage nanofiltration membranes in the S3 are all roll type ultrafiltration membranes, and the molecular weight cut-off of the first-stage nanofiltration membrane is 500 Da; the molecular weight cut-off of the secondary nanofiltration membrane is 150 Da; controlling the pressure range of the continuous nanofiltration membrane device to be 5.0MPa, controlling the temperature to be 45 ℃, controlling the pressure range before the membrane of the continuous nanofiltration membrane device to be 5.0MPa, controlling the pH value to be 9.5 in the primary nanofiltration process and the secondary nanofiltration process, and controlling the time to be 60 min;
in the S4, the concentration temperature is 80 ℃, and the vacuum degree is 0.1 MPa;
in S5, the concentration temperature is 70 ℃, and the vacuum degree is 0.1 MPa.
Effect of the experiment
The yield of the crude polysaccharide was determined by phenol-sulfuric acid method (polysaccharide content g/raw material weight g.times.100%), and the betaine content in the lyophilized crude product was determined by HPLC method (betaine content g/crude product weight/g.times.100%). Comparing the yield of each single-factor process and the yield of the thermal flocculation combined nanofiltration process to obtain the following table 2:
TABLE 2 yield of beet polysaccharide and betaine content in different processes
After the exudate is treated by thermal flocculation, macromolecular substances such as pectin and the like are separated out from the feed liquid due to unstable colloids, so that the sedimentation performance of the exudate is improved, the pectin content is greatly reduced, and the condition that other degradation products flow into a next working section to influence the subsequent process and the product quality is avoided. However, the flocculation has no influence on micromolecular substances in the exudate, such as monosaccharide, micromolecular pigment and the like, micromolecular sugar and polysaccharide substances enter an ultrafiltration stage together and are filtered out as filtrate together, and the function of separating polysaccharide and betaine cannot be achieved, so that the polysaccharide yield measured by a phenol-sulfuric acid method is higher, and the content of betaine is lower. When only nanofiltration is carried out, a large amount of pectin in the ultrafiltration stage is partially dissolved in water and partially exists in a suspended state and wraps a large amount of easily-settled solids, so that a large amount of pectin is intercepted by the ultrafiltration membrane, the flux of the ultrafiltration membrane is low, the efficiency is low, and finally the polysaccharide interception rate of a nanofiltration section is low and the impurity content is high. The invention adopts the process of combining the composite high-temperature thermal flocculant and the nanofiltration membrane, can continuously separate beet polysaccharide and betaine from beet exudation juice, has high yield and low cost, reduces membrane pressure, prolongs the service life of the membrane, and is suitable for durable process requirements.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for separating and concentrating beet polysaccharide and betaine by using thermal flocculation combined with a multi-stage nanofiltration membrane is characterized by comprising the following steps:
s1, pretreatment: using water as an extracting solution for beet, and carrying out exudation and impurity removal to obtain a beet juice leaching solution;
s2, thermal flocculation: mixing the beet juice leachate obtained in the step S1 with a composite high-temperature flocculant, heating to obtain floccules, and performing inclined plate sedimentation to obtain a supernatant;
s3, clarifying and decoloring: clarifying the supernatant in the S2 by an ultrafiltration membrane and decoloring by active carbon to obtain feed liquid;
s4, continuous nanofiltration membrane process: placing the feed liquid in a continuous nanofiltration membrane device, and performing primary nanofiltration to obtain trapped fluid 1 and permeate fluid 1, wherein the trapped fluid 1 is polysaccharide concentrated solution; the permeate 1 enters secondary nanofiltration to obtain trapped fluid 2 and permeate 2, wherein the permeate 2 is a betaine concentrated solution, and the trapped fluid 2 is a sucrose concentrated solution;
s5, polysaccharide concentration: concentrating the trapped fluid 1, and freeze-drying;
s6 betaine concentration: the permeate 2 was concentrated and freeze-dried.
2. The method of claim 1, wherein the composition of the composite high temperature flocculant of step S2: the mass ratio of polyacrylamide to polysilicic acid is 1: 1, mixing; the addition amount of the composite high-temperature flocculant is 3-5 ppm.
3. The method of claim 2, wherein the heating of step S2 is carried out to 80-85 ℃ for 15-20 min; the time of inclined plate sedimentation is 20-30 min.
4. The method of claim 3, wherein the inclined plate sedimentation in step S2 is at least 300m3Water inflow of/h and 270m3Water yield per hour.
5. The method of claim 1, wherein the pore size of the ultrafiltration membrane in step S3 is 15 to 20kDa, and the pressure after membrane is controlled at 0.2 to 0.3 Mpa; and decolorizing the activated carbon, controlling the pH to be stable at 9-10, stabilizing the temperature at 45-55 ℃, and controlling the time to be 15-20 min.
6. The method of claim 1, wherein the molecular weight cut-off of the primary nanofiltration membrane in step S4 is 200-800 Da; the molecular weight cut-off of the secondary nanofiltration membrane is more than or equal to 150Da and less than 200 Da; and controlling the pressure range before the membrane of the continuous nanofiltration membrane device to be 1.0-8.0 MPa, controlling the temperature to be 35-55 ℃, controlling the pH value to be 9-10 in the primary nanofiltration and secondary nanofiltration processes, and controlling the time to be 60-90 min.
7. The method of claim 6, wherein the continuous nanofiltration membrane unit of the step S4 has a pre-membrane pressure of 3.0MPa and a temperature of 55 ℃.
8. The method of claim 1, wherein the concentration temperature in step S5 is 75 to 80 ℃ and the vacuum degree is 0.1 to 0.2 MPa.
9. The method of claim 1, wherein the concentration temperature in step S6 is 70-80 ℃ and the vacuum degree is 0.1-0.2 MPa.
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| CN115852065A (en) * | 2022-10-14 | 2023-03-28 | 广西新蜜技制糖有限责任公司 | Method for preparing white sugar by squeezing sugarcane |
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