CN113248551B - System and method for preparing refined xylose by utilizing xylose mother liquor chromatographic extract - Google Patents
System and method for preparing refined xylose by utilizing xylose mother liquor chromatographic extract Download PDFInfo
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- CN113248551B CN113248551B CN202110568200.7A CN202110568200A CN113248551B CN 113248551 B CN113248551 B CN 113248551B CN 202110568200 A CN202110568200 A CN 202110568200A CN 113248551 B CN113248551 B CN 113248551B
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- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
Abstract
The invention relates to a system for preparing refined xylose by utilizing xylose mother liquor chromatographic extract, which comprises a pre-evaporation tank, a primary evaporator, a primary decolorizing tank, an ion exchange column, a secondary evaporator, a crystallization tank, a primary centrifugal machine, a dissolving tank, a secondary decolorizing tank, a tertiary evaporator, a vacuum sugar boiling tank, a crystallization tank, a secondary centrifugal machine, a dryer and a sieving machine, wherein the xylose mother liquor chromatographic extract is stored in the pre-evaporation tank, the secondary centrifugal machine is used for carrying out centrifugal treatment to obtain secondary mother liquor and secondary massecuite, the primary decolorizing tank is used for carrying out decolorizing treatment on the mixed liquor of concentrated solution and secondary mother liquor obtained after the primary evaporator is evaporated and concentrated, and the sieving machine is used for sieving the secondary massecuite obtained after the dryer is used for drying so as to obtain refined xylose. The invention also discloses a method for preparing refined xylose by utilizing the xylose mother liquor chromatographic extract of the system. The invention reduces the problems of excessive quality, energy waste and the like in the xylose refining production process, and reduces the production cost of enterprises.
Description
Technical Field
The invention belongs to the technical field of xylose preparation, and particularly relates to a system and a method for preparing refined xylose by utilizing xylose mother liquor chromatographic extract.
Background
Xylose is a white crystal or fine powder, and is one of important sugar alcohol sugar substitute products. Xylose is absorbed by the intestines after entering the human body, but 90% of xylose is not utilized and directly discharged from the body due to the lack of enzyme systems for metabolizing xylose, and the symptoms such as diarrhea and abdominal distension of the human body are avoided. Therefore, the method has been widely applied to the production of baked foods, biscuits, rice fruits, ham, sausage, bacon and the like. However, xylose, which is common in the market, is unfavorable for processing in downstream industries due to the disadvantages of fine particles, difficult flowability, yellow color, easy caking, poor storage stability and the like, so the demand for refining xylose is increasing.
The current xylose refining production is carried out by dissolving common xylose, refining, removing impurities, ion exchanging, concentrating, crystallizing, and the like. The indexes of physicochemical property, granularity and the like are better than those of common xylose. For example, chinese patent publication No. CN112358511A discloses a process for producing refined xylose, which takes crystalline xylose as a raw material, and produces refined xylose with higher purity, larger granularity and higher cleanliness through the steps of redissolving, filtering, concentrating, crystallizing, drying and the like. However, the process has the following disadvantages: (1) The content of the common xylose is more than 98.5%, the moisture is less than 0.3%, and the common xylose is used as a raw material to produce refined xylose, so that the quality waste and the energy consumption are large; (2) The common xylose is used as the raw material for production, and the crystallization speed is too high due to the high purity of the xylose, so that the crystallization effect is difficult to ensure; (3) The crystal grain size control stability is poor by adopting a cooling crystallization mode for production.
On the other hand, the secondary mother liquor of xylose is generally treated as waste material and has low utilization value.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a system and a method for preparing refined xylose by utilizing the xylose mother liquor chromatographic extract, so that the quality and energy waste are reduced, the production process is easy to control, and the purity of the xylose is high. Meanwhile, xylose is prepared by utilizing the secondary mother liquor of xylose, so that the utilization rate and the utilization value of the secondary mother liquor are improved.
The invention is realized by the way, the system for preparing refined xylose by utilizing the xylose mother liquor chromatographic extract comprises a pre-evaporation tank, a primary evaporator, a primary decolorizing tank, an ion exchange column, a secondary evaporator, a crystallization tank, a primary centrifugal machine, a dissolving tank, a secondary decolorizing tank, a tertiary evaporator, a vacuum sugar boiling tank, a crystallization tank, a secondary centrifugal machine, a dryer and a screening machine which are communicated in sequence through pipelines, wherein the xylose mother liquor chromatographic extract is stored in the pre-evaporation tank, the primary evaporator is used for carrying out evaporation concentration treatment on the xylose mother liquor chromatographic extract, the dissolving tank is used for carrying out redissolution treatment on primary massecuite after centrifugal treatment of the primary centrifugal machine, the secondary centrifugal machine is used for carrying out secondary centrifugal treatment on vacuum crystal materials obtained by the vacuum sugar boiling tank and the crystallization tank to obtain secondary mother liquor and secondary massecuite, the primary decolorizing tank is used for carrying out decolorizing filtration treatment on mixed liquor of concentrated solution and secondary mother liquor after the evaporation concentration treatment of the primary evaporator, the dryer is used for drying the secondary massecuite, and the screening machine is used for carrying out screening treatment on the secondary massecuite after the drying treatment of the dryer to obtain refined xylose finished product.
Further, the system further comprises a raw material tank, a front decolorizing tank, a front ion exchange column and a chromatographic column which are communicated through pipelines in sequence, wherein the raw material tank is used for storing xylose mother liquor, a feed inlet of the raw material tank is communicated with a discharge outlet of a primary centrifugal machine, the raw material tank is used for further storing primary mother liquor obtained after centrifugal treatment of the primary centrifugal machine, a discharge end of the chromatographic column is communicated with a feed end of the front evaporating tank through the pipelines, and the front evaporating tank is used for storing xylose mother liquor chromatographic extract after chromatographic separation treatment of the chromatographic column.
Further, the primary evaporator is an MVR evaporator.
Further, the secondary evaporator is a four-effect evaporator.
Further, the triple evaporator is a triple effect evaporator.
The present invention is thus achieved by providing a method for producing refined xylose using a xylose mother liquor chromatographic extract, which uses the system for producing refined xylose using a xylose mother liquor chromatographic extract as described above, the method comprising the steps of:
step 1, performing primary evaporation concentration treatment on xylose mother liquor chromatographic extract, concentrating until the refraction is 40% -50%, and discharging, wherein the concentration of the xylose mother liquor chromatographic extract is 15% -20%, and the xylose content is 70% -80%;
step 2, mixing the material obtained in the step 1 with the secondary mother solution obtained in the step 7 according to the volume ratio of 2:1-3:1, performing primary decoloring and filtering treatment, and discharging after obtaining a material with the light transmission of more than 60%;
step 3, discharging the material obtained in the step 2 after ion exchange treatment;
step 4, carrying out secondary evaporation concentration treatment on the material obtained in the step 3, concentrating to 75% -85% of refraction, then sequentially carrying out primary cooling crystallization and primary centrifugal separation treatment, returning primary mother liquor obtained by primary centrifugal separation to a raw material tank for standby, conveying primary massecuite with 90% -95% of xylose content obtained by primary centrifugal separation to a dissolving tank for re-dissolving treatment, and discharging after refraction control is carried out by 40% -50%;
step 5: sequentially carrying out secondary decolorization and filtration and tertiary evaporation and concentration treatment on the material obtained in the step 4, concentrating until the concentration is 70% -75%, and discharging;
step 6: sequentially carrying out vacuum crystallization and secondary cooling crystallization treatment on the material obtained in the step 5, enabling the material to enter a vacuum sugar boiling tank, concentrating the material to be crystallized in a vacuum environment, and cooling and crystallizing according to a certain temperature gradient;
step 7: carrying out secondary centrifugal separation treatment on the material obtained in the step 6, returning secondary mother liquor obtained by separation to be mixed with the discharged material obtained in the step 1, and temporarily storing secondary massecuite obtained by secondary separation in a pre-drying tank;
step 8: and (3) sequentially drying and screening the secondary massecuite obtained in the step (7) to obtain refined xylose crystals.
Further, the xylose mother liquor chromatographic extract is obtained by removing impurities from xylose mother liquor with the xylose content of 40% -50% stored in a raw material tank through a decoloring and ion exchange procedure and then performing chromatographic separation treatment.
Further, in step 3, the pH of the discharged material after the ion exchange treatment is controlled to be above 3.5, and the conductivity is less than 50us/cm.
Compared with the prior art, the system and the method for preparing refined xylose by utilizing the xylose mother liquor chromatographic extract have the following characteristics:
1. the process related by the invention has lower carbon footprint than the prior process, and is a green low-carbon process;
2. according to the invention, only one-time drying is needed from raw materials to xylose refining, so that the energy consumption in the production process is greatly reduced, and the production cost is reduced;
3. the invention adopts the vacuum crystallization and cooling crystallization mode to produce, the xylose crystallization process is more stable, and the granularity of the xylose finished product is more uniform;
4. in the process, the purity of the material in the redissolution process is controlled to be 90% -95%, and compared with the prior art, the quality waste is reduced, the production efficiency is improved, and the cost is reduced;
5. the secondary mother liquor obtained by secondary centrifugal separation is mixed with the material after primary evaporation and concentration for primary decolorization and filtration, so that the secondary mother liquor is fully utilized, and the utilization rate and the utilization value of the secondary mother liquor are improved.
Drawings
FIG. 1 is a schematic diagram of the method for preparing refined xylose by using xylose mother liquor chromatographic extract.
Description of the embodiments
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to FIG. 1, a preferred embodiment of the system for producing refined xylose from xylose mother liquor chromatographic extract according to the present invention is shown, wherein the arrowed lines indicate the flow direction of the material in the system of the present invention. The system comprises a pre-evaporation tank 1, a primary evaporator 2, a primary decoloring tank 3, an ion exchange column 4, a secondary evaporator 5, a crystallization tank 6, a primary centrifugal machine 7, a dissolving tank 8, a secondary decoloring tank 9, a tertiary evaporator 10, a vacuum sugar boiling tank and crystallization tank 11, a secondary centrifugal machine 12, a dryer 13 and a screening machine 14 which are communicated through pipelines in sequence. The system further comprises a raw material tank 15, a front decolorizing tank 16, a front ion exchange column 17 and a chromatographic column 18 which are communicated with each other through pipelines in sequence.
The xylose mother liquor chromatographic extract A is stored in a pre-evaporation tank 1, and a primary evaporator 2 is used for evaporating and concentrating the xylose mother liquor chromatographic extract A. The primary decolorization tank 3 is used for decolorizing and filtering the mixed solution of the concentrated solution obtained by evaporating and concentrating the primary evaporator 2 and the secondary mother solution B. The ion exchange column 4 is used for carrying out ion purification treatment on the material after the decolorization and filtration treatment to remove metal ions in the material. The secondary evaporator 5 is used for concentrating the material after the ion purification treatment. The crystallization cylinder 6 is used for crystallizing the concentrated material of the secondary evaporator 5.
The primary centrifuge 7 is for centrifuging the crystallized material obtained in the crystallization tank 6 to obtain a primary mother liquor C and a primary massecuite D, respectively. The dissolving tank 8 is used for redissolving the primary massecuite D after the centrifugal treatment by the primary centrifuge 7. The secondary decolorizing tank 9 is used for filtering the sugar solution after the re-dissolving treatment to remove impurities and foreign matters. The material after decolorization is concentrated by the triple evaporator 10. The vacuum sugar boiling tank and the crystallization tank 11 are used for carrying out vacuum crystallization treatment on the concentrated material. The secondary centrifuge 12 is used for carrying out secondary centrifugation treatment on the vacuum crystallization materials obtained by the vacuum sugar boiling tank and the crystallization tank 11 to obtain secondary mother liquor B and secondary massecuite E, the dryer 13 is used for drying the secondary massecuite E, and the sieving machine 14 is used for sieving the secondary massecuite E after the drying treatment of the dryer 13 to obtain a refined xylose G finished product.
The feed tank 15 is used for storing xylose mother liquor F. One feed inlet of the raw material tank 15 is communicated with one discharge outlet of the primary centrifugal machine 7, and the raw material tank 15 also stores primary mother liquor C obtained after centrifugal treatment of the primary centrifugal machine 7. The front decolorizing tank 16 and the front ion exchange column 17 are respectively used for carrying out impurity removal treatment on the xylose mother liquor F. The discharge end of the chromatographic column 18 is communicated with the feed end of the evaporation front tank 1 through a pipeline. The pre-evaporation tank 1 is used for storing xylose mother liquor chromatographic extract A after chromatographic separation treatment by a chromatographic column 18.
In this embodiment, the primary evaporator 2 is an MVR evaporator, the secondary evaporator 5 is a four-effect evaporator, and the tertiary evaporator 10 is a three-effect evaporator.
Referring to FIG. 1, the invention also discloses a method for preparing refined xylose by utilizing the xylose mother liquor chromatographic extract, which uses the system for preparing refined xylose by utilizing the xylose mother liquor chromatographic extract. The method comprises the following steps:
and step 1, performing primary evaporation concentration treatment on the xylose mother liquor chromatographic extract A, concentrating until the refraction is 40% -50%, and discharging, wherein the concentration of the xylose mother liquor chromatographic extract A is 15% -20%, and the xylose content is 70% -80%.
And 2, mixing the material obtained in the step 1 with the secondary mother solution B obtained in the step 7 according to the volume ratio of 2:1-3:1, performing primary decoloring and filtering treatment, and discharging after obtaining a material with the light transmission of more than 60%.
And 3, carrying out ion exchange treatment on the materials obtained in the step 2, and discharging.
And 4, carrying out secondary evaporation concentration treatment on the material obtained in the step 3, concentrating to 75% -85% of refraction, then sequentially carrying out primary cooling crystallization and primary centrifugal separation treatment, returning the primary mother liquor C obtained by centrifugal separation to the raw material tank 15 for standby, conveying the primary massecuite D with 90% -95% of xylose content obtained by centrifugal separation to the dissolution tank 8 for re-dissolution treatment, and discharging after controlling the refraction to 40% -50%.
Step 5: and (3) sequentially carrying out secondary decolorization filtration and tertiary evaporation concentration treatment on the material obtained in the step (4), concentrating to 70% -75% concentration, and discharging.
Step 6: and 5, sequentially carrying out vacuum crystallization and secondary cooling crystallization treatment on the material obtained in the step 5, feeding the material into a vacuum sugar boiling tank, concentrating the material to be crystallized in a vacuum environment, and cooling and crystallizing according to a certain temperature gradient.
Step 7: and (3) carrying out secondary centrifugal separation treatment on the material obtained in the step (6), returning the separated secondary mother liquor B to the system, mixing with the material obtained in the step (1), and feeding the wet sugar obtained in the separation into a pre-drying tank for temporary storage.
Step 8: and (3) sequentially drying and screening the secondary massecuite E obtained in the step (7) to obtain refined xylose G crystals, wherein the moisture content of the xylose crystals is controlled to be less than 0.3%.
Specifically, the xylose mother liquor chromatographic extract A is obtained by removing impurities from xylose mother liquor with the xylose content of 40% -50% stored in a raw material tank through a decoloring and ion exchange procedure and then performing chromatographic separation treatment.
Specifically, in the step 3, the pH of the discharged material after the ion exchange treatment is controlled to be more than 3.5, and the conductivity is less than 50us/cm.
The process of the invention is further illustrated below in connection with specific examples.
Examples
Referring again to FIG. 1, a first embodiment of the method for producing refined xylose using a xylose mother liquor chromatographic extract of the present invention comprises the steps of:
step 11, primary evaporation concentration: and (3) conveying the xylose mother liquor chromatographic extract A with the concentration of 17% to an MVR evaporator through a pump, concentrating to have the refraction of 40% -50%, and discharging to improve the decoloring effect.
Wherein, in the xylose mother liquor chromatographic extract A, the xylose content is 75.39%, the glucose is 4.48%, the galactose is 2.32%, the arabinose is 4.93%, the mannose is 7.34% and the other miscellaneous sugar is 4.43%.
Step 12, primary decoloring and filtering: mixing the material obtained in the step 11 with the secondary mother solution B obtained in the step 111 according to a volume ratio of 3:1, mixing, adding into a plate-frame filtering front tank, adding 1% (weight-volume ratio) active carbon, mixing at 65deg.C for 30min, filtering with a plate frame, and removing pigment and impurities to obtain material with light transmission of more than 60%.
Step 13, ion exchange: and (3) purifying the material obtained in the step (12) by an ion exchange column to remove metal ions in the material, wherein the pH value of the discharged material is controlled to be more than 3.5, and the conductivity is less than 50us/cm.
Step 14: secondary evaporation concentration: and (3) feeding the material obtained in the step (13) into a four-effect evaporator, lifting the concentration of the material to 75% -85% by utilizing steam, and discharging the material to a crystallization cylinder after the concentration is qualified.
Step 15: and (3) primary cooling crystallization: and (3) cooling the material obtained in the step (14), wherein the initial temperature starts to be cooled according to the range of 0.5-1 ℃ per hour in the period of reducing the initial temperature to 50 ℃, and the temperature is increased according to the range of 1-2 ℃ per hour in the period of reducing the initial temperature to 25 ℃.
Step 16: primary centrifugation and massecuite redissolution: and (3) discharging the material obtained in the step (15) into a centrifugal machine through a packing auger for centrifugal treatment, wherein the centrifugal speed is 1150rpm, and the centrifugal period is 30-45 min. And (3) returning the primary mother liquor C obtained by centrifugal separation to a raw material tank 15 for standby through the action of centrifugal force, conveying the primary massecuite D with the xylose content of 90% -95% to a dissolving tank 8 through a packing auger for redissolution, adding purified water, dissolving into concentrated liquid with the refraction of 40% -50%, and discharging.
Step 17: secondary decolorization and filtration: and (3) carrying out secondary decoloring treatment on the material obtained in the step (16), adding activated carbon with the mass-volume ratio of 0.5% for decoloring, controlling the light transmittance of discharged material to be more than 90%, and filtering the material qualified in light transmittance through a filter element with the size of 0.45 microns to reduce the risk of foreign matters in the material.
Step 18: and (3) three times of evaporation concentration: and (3) feeding the material obtained in the step (17) into a triple-effect evaporator, concentrating to 70% -75% of concentration, and discharging.
Step 19: vacuum crystallization: and (3) feeding the material obtained in the step (18) into a vacuum sugar boiling tank, introducing steam in a vacuum environment with the vacuum degree of-0.095 MPa, controlling the temperature to be 60-70 ℃, concentrating until the material is crystallized, stopping adding steam, and keeping the vacuum state for continuous concentration until the crystallization is finished.
Step 110: and (3) secondary cooling crystallization: and (3) carrying out secondary cooling crystallization on the material obtained in the step (19), maintaining the initial temperature for 1-2 h, then starting cooling, maintaining the cooling range of 0.5-1 ℃ per hour when the initial temperature is reduced to 50 ℃, and maintaining the cooling range of 1-2 ℃ per hour when the temperature is reduced to 25 ℃.
Step 111: secondary centrifugal separation: and (3) carrying out secondary centrifugal separation on the material obtained in the step (110) by using a centrifugal machine, wherein the centrifugal maximum rotating speed is 1150rpm, adding purified water at 50 ℃ in the centrifugal process to clean the surface of massecuite, and removing mother liquor attached to the surface of crystals. And (3) returning the separated secondary mother liquor B to the system to be mixed with the material obtained in the step (11), and enabling the separated secondary massecuite E to enter a pre-drying tank for temporary storage.
Step 112: and (3) drying: and (3) drying the secondary massecuite E obtained in the step (111) in a hot air environment to obtain xylose crystals, wherein the moisture content is controlled to be less than 0.3%.
Step 113: screening and packaging a finished product: the xylose crystals are conveyed to a sieving machine 14 for sieving through air flow, and the sieved xylose crystals are packaged into finished products of refined xylose G after being monitored by equipment such as a magnetic rod, a gold detector and the like.
The xylose physical and chemical indexes (including pH, light transmittance, ash content, and the like) and sensory indexes (including whiteness, color, granularity, templates, foreign matters, and the like) of the finished product of the refined xylose prepared in the embodiment 1 can meet the requirements of refined xylose, and meanwhile, the method can reduce the problems of excessive quality, energy waste, high carbon footprint, difficult process control, and the like in the production process of the refined xylose, thereby reducing the production cost of enterprises and meeting the requirements of green low carbon.
Examples
Referring again to FIG. 1, a second embodiment of the method for producing refined xylose using a xylose mother liquor chromatographic extract of the present invention comprises the steps of:
step 21, primary evaporation concentration: and (3) conveying the xylose mother liquor chromatographic extract A with the concentration of 15% to an MVR evaporator through a pump, concentrating to have the refraction of 40% -50%, and discharging to improve the decoloring effect.
Wherein, in the xylose mother liquor chromatographic extract A, the xylose content is 75.39%, the glucose is 4.48%, the galactose is 2.32%, the arabinose is 4.93%, the mannose is 7.34% and the other miscellaneous sugar is 4.43%.
Step 22, primary decoloring and filtering: mixing the material obtained in the step 21 with the secondary mother solution B obtained in the step 211 according to a volume ratio of 2:1, mixing, adding into a plate-frame filtering front tank, adding 1% (weight-volume ratio) active carbon, mixing at 65deg.C for 30min, filtering with a plate frame, and removing pigment and impurities to obtain material with light transmission of more than 60%.
Step 23, ion exchange: and (2) purifying the material obtained in the step (22) by an ion exchange column to remove metal ions in the material, wherein the pH value of the discharged material is controlled to be more than 3.5, and the conductivity is less than 50us/cm.
Step 24: secondary evaporation concentration: and (3) feeding the material obtained in the step (23) into a four-effect evaporator, lifting the concentration of the material to 75% -85% by utilizing steam, and discharging the material to a crystallization cylinder after the concentration is qualified.
Step 25: and (3) primary cooling crystallization: and (3) cooling the material obtained in the step 24, wherein the initial temperature starts to be cooled according to the range of 0.5-1 ℃ per hour in the period of reducing the initial temperature to 50 ℃, and the temperature is increased according to the range of 1-2 ℃ per hour in the period of reducing the initial temperature to 25 ℃.
Step 26: primary centrifugation and massecuite redissolution: and (3) discharging the material obtained in the step (25) into a centrifugal machine through a packing auger for centrifugal treatment, wherein the centrifugal speed is 1150rpm, and the centrifugal period is 30-45 min. And (3) returning the primary mother liquor C obtained by centrifugal separation to a raw material tank 15 for standby through the action of centrifugal force, conveying the primary massecuite D with the xylose content of 90% -95% to a dissolving tank 8 through a packing auger for redissolution, adding purified water, dissolving into concentrated liquid with the refraction of 40% -50%, and discharging.
Step 27: secondary decolorization and filtration: and (5) carrying out secondary decoloring treatment on the material obtained in the step (26), adding activated carbon with the mass-volume ratio of 0.5% for decoloring, controlling the light transmittance of discharged material to be more than 90%, and filtering the material qualified in light transmittance through a filter element with the size of 0.45 microns to reduce the risk of foreign matters in the material.
Step 28: and (3) three times of evaporation concentration: and (3) feeding the material obtained in the step (27) into a triple-effect evaporator, concentrating to 70% -75% of concentration, and discharging.
Step 29: vacuum crystallization: and (3) feeding the material obtained in the step (28) into a vacuum sugar boiling tank, introducing steam in a vacuum environment with the vacuum degree of-0.095 MPa, controlling the temperature to be 60-70 ℃, concentrating until the material is crystallized, stopping adding steam, and keeping the vacuum state for continuous concentration until the crystallization is finished.
Step 210: and (3) secondary cooling crystallization: and (3) carrying out secondary cooling crystallization on the material obtained in the step (29), maintaining the initial temperature for 1-2 h, then starting cooling, maintaining the cooling range of 0.5-1 ℃ per hour when the initial temperature is reduced to 50 ℃, and maintaining the cooling range of 1-2 ℃ per hour when the temperature is reduced to 25 ℃.
Step 211: secondary centrifugal separation: and (2) carrying out secondary centrifugal separation on the material obtained in the step (210) by using a centrifugal machine, wherein the centrifugal maximum rotating speed is 1150rpm, adding purified water with the temperature of 50 ℃ in the centrifugal process to clean the surface of massecuite, and removing mother liquor attached to the surface of crystals. And (3) returning the separated secondary mother liquor B to the system to be mixed with the material obtained in the step (21), and enabling the separated secondary massecuite E to enter a pre-drying tank for temporary storage.
Step 212: and (3) drying: and (3) drying the secondary massecuite E obtained in the step 211 in a hot air environment to obtain xylose crystals, wherein the moisture content is controlled to be less than 0.3%.
Step 213: screening and packaging a finished product: the xylose crystals are conveyed to a sieving machine 14 for sieving through air flow, and the sieved xylose crystals are packaged into finished products of refined xylose G after being monitored by equipment such as a magnetic rod, a gold detector and the like.
Examples
Referring again to FIG. 1, a third embodiment of the method for producing refined xylose using a xylose mother liquor chromatographic extract of the present invention comprises the steps of:
step 31, primary evaporation concentration: and (3) conveying the xylose mother liquor chromatographic extract A with the concentration of 20% to an MVR evaporator through a pump, concentrating to have the refraction of 40% -50%, and discharging to improve the decoloring effect.
Step 32, primary decoloring and filtering: mixing the material obtained in the step 31 with the secondary mother solution B obtained in the step 311 according to a volume ratio of 5:2, mixing, adding into a plate-frame filtering front tank, adding 1% (weight-volume ratio) active carbon, mixing at 65deg.C for 30min, filtering with a plate frame, and removing pigment and impurities to obtain material with light transmission of more than 60%.
Step 33, ion exchange: and (3) purifying the material obtained in the step (32) by an ion exchange column to remove metal ions in the material, wherein the pH value of the discharged material is controlled to be more than 3.5, and the conductivity is less than 50us/cm.
Step 34: secondary evaporation concentration: and (3) feeding the material obtained in the step (33) into a four-effect evaporator, lifting the concentration of the material to 75% -85% by utilizing steam, and discharging the material to a crystallization cylinder after the concentration is qualified.
Step 35: and (3) primary cooling crystallization: and (3) cooling the material obtained in the step (34), wherein the initial temperature starts to be cooled according to the range of 0.5-1 ℃ per hour in the period of reducing the initial temperature to 50 ℃, and the temperature is increased according to the range of 1-2 ℃ per hour in the period of reducing the initial temperature to 25 ℃.
Step 36: primary centrifugation and massecuite redissolution: and (3) discharging the material obtained in the step (35) into a centrifugal machine through a packing auger for centrifugal treatment, wherein the centrifugal speed is 1150rpm, and the centrifugal period is 30-45 min. And (3) returning the primary mother liquor C obtained by centrifugal separation to a raw material tank 15 for standby through the action of centrifugal force, conveying the primary massecuite D with the xylose content of 90% -95% to a dissolving tank 8 through a packing auger for redissolution, adding purified water, dissolving into concentrated liquid with the refraction of 40% -50%, and discharging.
Step 37: secondary decolorization and filtration: and (3) carrying out secondary decoloring treatment on the material obtained in the step 36, adding activated carbon with the mass-volume ratio of 0.5% for decoloring, controlling the light transmittance of discharged material to be more than 90%, and filtering the material qualified in light transmittance through a filter element with the size of 0.45 microns to reduce the risk of foreign matters in the material.
Step 38: and (3) three times of evaporation concentration: and (3) feeding the material obtained in the step (37) into a triple-effect evaporator, concentrating to 70% -75% of concentration, and discharging.
Step 39: vacuum crystallization: and (3) feeding the material obtained in the step 38 into a vacuum sugar boiling tank, introducing steam in a vacuum environment with the vacuum degree of-0.095 MPa, controlling the temperature to be 60-70 ℃, stopping adding steam after concentrating until the material is crystallized, keeping the vacuum state, continuing concentrating until the crystallization is finished, and discharging to a crystallization cylinder.
Step 310: and (3) secondary cooling crystallization: and (3) carrying out secondary cooling crystallization on the material obtained in the step (39), maintaining the initial temperature for 1-2 h, then starting cooling, maintaining the cooling range of 0.5-1 ℃ per hour when the initial temperature is reduced to 50 ℃, and maintaining the cooling range of 1-2 ℃ per hour when the temperature is reduced to 25 ℃.
Step 311: secondary centrifugal separation: and (3) carrying out secondary centrifugal separation on the material obtained in the step 310 by using a centrifugal machine, wherein the highest centrifugal speed is 1150rpm, adding purified water at 50 ℃ in the centrifugal process to clean the surface of massecuite, and removing mother liquor attached to the surface of crystals. And (3) returning the separated secondary mother liquor S to the system for mixing with the material obtained in the step (31), and enabling the separated secondary massecuite E to enter a pre-drying tank for temporary storage.
Step 312: and (3) drying: and (3) drying the secondary massecuite E obtained in the step 311 in a hot air environment to obtain xylose crystals, wherein the moisture content is controlled to be less than 0.3%.
Step 313: screening and packaging a finished product: the xylose crystals are conveyed to a sieving machine 14 for sieving through air flow, and the sieved xylose crystals are packaged into finished products of refined xylose G after being monitored by equipment such as a magnetic rod, a gold detector and the like.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (8)
1. A system for preparing refined xylose by utilizing xylose mother liquor chromatographic extract is characterized by comprising an evaporation front tank, a primary evaporator, a primary decolorizing tank, an ion exchange column, a secondary evaporator, a crystallization tank, a primary centrifugal machine, a dissolving tank, a secondary decolorizing tank, a tertiary evaporator, a vacuum sugar boiling tank, a crystallization tank, a secondary centrifugal machine, a dryer and a sieving machine which are communicated through pipelines in sequence, wherein the xylose mother liquor chromatographic extract is stored in the evaporation front tank, the primary evaporator is used for carrying out evaporation concentration treatment on the xylose mother liquor chromatographic extract, the dissolving tank is used for carrying out re-dissolution treatment on primary massecuite obtained after the centrifugal treatment of the primary centrifugal machine, the secondary centrifugal machine is used for carrying out secondary centrifugal treatment on vacuum crystal materials obtained by the vacuum sugar boiling tank and the crystallization tank to obtain secondary mother liquor and secondary massecuite, the primary decolorizing tank is used for carrying out decolorizing filtration treatment on mixed liquor of concentrated solution obtained after the evaporation concentration treatment of the primary evaporator and the secondary mother liquor, the dryer is used for drying the secondary massecuite, and the sieving machine is used for sieving the secondary massecuite obtained after the drying treatment of the dryer to obtain refined xylose finished products.
2. The system for producing refined xylose by utilizing xylose mother liquor chromatographic extract as claimed in claim 1, further comprising a raw material tank, a front decolorizing tank, a front ion exchange column and a chromatographic column which are communicated sequentially through a pipeline, wherein the raw material tank is used for storing xylose mother liquor, one feed inlet of the raw material tank is communicated with one discharge outlet of a primary centrifuge, the raw material tank is also used for storing primary mother liquor obtained after centrifugal treatment of the primary centrifuge, the discharge end of the chromatographic column is communicated with the feed end of the evaporation front tank through a pipeline, and the evaporation front tank is used for storing xylose mother liquor chromatographic extract after chromatographic separation treatment of the chromatographic column.
3. The system for producing refined xylose by utilizing xylose mother liquor chromatographic extract as claimed in claim 1, characterized in that said primary evaporator is a MVR evaporator.
4. The system for producing refined xylose by utilizing xylose mother liquor chromatographic extract as claimed in claim 1, wherein said secondary evaporator is a four-effect evaporator.
5. The system for producing refined xylose by utilizing xylose mother liquor chromatographic extract as claimed in claim 1, characterized in that said triple evaporator is a triple effect evaporator.
6. A method for producing xylose by using the xylose mother liquor chromatographic extract, which uses the system for producing xylose by using the xylose mother liquor chromatographic extract as claimed in any one of claims 1 to 5, characterized in that it comprises the steps of:
step 1, performing primary evaporation concentration treatment on xylose mother liquor chromatographic extract, concentrating until the refraction is 40% -50%, and discharging, wherein the concentration of the xylose mother liquor chromatographic extract is 15% -20%, and the xylose content is 70% -80%;
step 2, mixing the material obtained in the step 1 with the secondary mother solution obtained in the step 7 according to the volume ratio of 2:1-3:1, performing primary decoloring and filtering treatment, and discharging after obtaining a material with the light transmission of more than 60%;
step 3, discharging the material obtained in the step 2 after ion exchange treatment;
step 4, carrying out secondary evaporation concentration treatment on the material obtained in the step 3, concentrating to 75% -85% of refraction, then sequentially carrying out primary cooling crystallization and primary centrifugal separation treatment, returning primary mother liquor obtained by primary centrifugal separation to a raw material tank for standby, conveying primary massecuite with 90% -95% of xylose content obtained by primary centrifugal separation to a dissolving tank for re-dissolving treatment, and discharging after refraction control is carried out by 40% -50%;
step 5: sequentially carrying out secondary decolorization and filtration and tertiary evaporation and concentration treatment on the material obtained in the step 4, concentrating until the concentration is 70% -75%, and discharging;
step 6: sequentially carrying out vacuum crystallization and secondary cooling crystallization treatment on the material obtained in the step 5, enabling the material to enter a vacuum sugar boiling tank, concentrating the material to be crystallized in a vacuum environment, and cooling and crystallizing according to a certain temperature gradient;
step 7: carrying out secondary centrifugal separation treatment on the material obtained in the step 6, returning secondary mother liquor obtained by separation to be mixed with the discharged material obtained in the step 1, and temporarily storing secondary massecuite obtained by secondary separation in a pre-drying tank;
step 8: and (3) sequentially drying and screening the secondary massecuite obtained in the step (7) to obtain refined xylose crystals.
7. The method for producing purified xylose by using a xylose mother liquor chromatographic extract as claimed in claim 6, wherein the xylose mother liquor chromatographic extract is obtained by subjecting xylose mother liquor having a xylose content of 40% -50% stored in a raw material tank to a decoloring and ion exchange process for removing impurities and then subjecting to chromatographic separation.
8. The method for producing xylose by using xylose mother liquor chromatographic extract as claimed in claim 6, characterized in that in step 3, the pH of the discharged material after ion exchange treatment is controlled to be 3.5 or more, and the conductivity is less than 50us/cm.
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| CN114105732B (en) * | 2021-12-27 | 2023-12-15 | 浙江华康药业股份有限公司 | Xylitol comprehensive utilization system and method thereof |
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| DE1643940A1 (en) * | 1967-09-05 | 1971-07-01 | Eickemeyer Rudolf Dipl Ing | Process and apparatus for the production of crystallized xylose |
| US6086681A (en) * | 1995-03-01 | 2000-07-11 | Xyrofin Oy | Method for recovery of xylose from solutions |
| CN109503676A (en) * | 2018-11-27 | 2019-03-22 | 浙江华康药业股份有限公司 | A method of preparing xylitol and mixing molasses from xylose mother liquid |
| CN112225762A (en) * | 2020-11-09 | 2021-01-15 | 安阳市豫鑫木糖醇科技有限公司 | Process for extracting xylose |
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| DE1643940A1 (en) * | 1967-09-05 | 1971-07-01 | Eickemeyer Rudolf Dipl Ing | Process and apparatus for the production of crystallized xylose |
| US6086681A (en) * | 1995-03-01 | 2000-07-11 | Xyrofin Oy | Method for recovery of xylose from solutions |
| CN109503676A (en) * | 2018-11-27 | 2019-03-22 | 浙江华康药业股份有限公司 | A method of preparing xylitol and mixing molasses from xylose mother liquid |
| CN112225762A (en) * | 2020-11-09 | 2021-01-15 | 安阳市豫鑫木糖醇科技有限公司 | Process for extracting xylose |
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