CN113387774A - Erythritol extraction process and system - Google Patents
Erythritol extraction process and system Download PDFInfo
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- CN113387774A CN113387774A CN202110594902.2A CN202110594902A CN113387774A CN 113387774 A CN113387774 A CN 113387774A CN 202110594902 A CN202110594902 A CN 202110594902A CN 113387774 A CN113387774 A CN 113387774A
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Abstract
The invention relates to the field of food, and discloses an extraction process of erythritol, which comprises the following steps of S1, ceramic membrane filtration, S2, nanofiltration filtration, S3, nanofiltration liquid classification treatment, S4, and concentration and crystallization. The invention also discloses an erythritol extraction system which comprises a primary ceramic membrane filtering device, a nanofiltration membrane purifying device, a resin separation purifying device and a concentration crystallization system which are mutually connected through pipelines. The nanofiltration dialysate outlet of the nanofiltration membrane purification device is provided with a grading device which can grade different outlets according to the concentration value of the nanofiltration dialysate, and the grading device is provided with a plurality of grading outlets. The invention adopts the grading device to grade the nanofiltration dialysate according to the solubility, and enters different treatment procedures according to different concentrations, thereby not only ensuring that the concentration change of the system is small, stabilizing the later process, but also greatly improving the utilization rate of the feed liquid, reducing the energy consumption of the subsequent evaporative crystallization, and simultaneously reducing the water consumption in the elution process.
Description
Technical Field
The invention relates to the field of food, in particular to an extraction process and system of erythritol.
Background
Erythritol is a newly developed 4-carbon sugar alcohol, can be prepared by fermentation of glucose, is a white crystalline powder, has a refreshing sweet taste, is less likely to absorb moisture, is stable at high temperatures, is stable in a wide PH range, has a mild cooling sensation when dissolved in the mouth, and is suitable as an additive for various foods. At present, the erythritol is produced by three main methods, namely a biological extraction method, a chemical synthesis method and a microbial fermentation method. In comparison, the microbial fermentation method is an ideal erythritol production method because of its mild production conditions, stable quality of target products, and high food safety.
The existing erythritol technology adopts fermentation liquor to pass through a set of ceramic membrane and continuously adds water for elution to improve the yield. The obtained dialysate passes through a nanofiltration membrane and is continuously added with water for elution so as to improve the yield. The main disadvantages of this process are: 1. the concentration of the feed liquid changes greatly, and the later process is unstable. 2. The concentration of the feed liquid is low, and the energy consumption of subsequent evaporation is high. 3. The water consumption is large.
Disclosure of Invention
The invention aims to provide an erythritol extraction process and system, wherein a grading device is adopted to grade nanofiltration dialysate according to the solubility, and different treatment procedures are performed according to different concentrations, so that the concentration change of the system is small, the later process is stabilized, the utilization rate of feed liquid is greatly improved, the energy consumption of subsequent evaporative crystallization is reduced, and the water consumption in the elution process is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses an extraction process of erythritol, which comprises the following steps:
s1, ceramic membrane filtration: eluting and filtering erythritol fermentation liquor through a first-stage ceramic membrane to obtain a first-stage dialysate and a first-stage concentrated solution, wherein the aperture of the first-stage ceramic membrane is 50-200 nm;
s2, nanofiltration and filtration: eluting and filtering the primary dialysate obtained in the step S1 by a nanofiltration membrane to obtain nanofiltration dialysate and nanofiltration concentrate, wherein the molecular weight cut-off of the nanofiltration membrane is 200 and 1000 daltons;
s3, nano-filtration liquid classification treatment: and (3) carrying out real-time detection on the erythritol concentration of the nanofiltration dialysate in the step S2, and carrying out classification treatment:
if the concentration of the nanofiltration dialysate is less than 13%, returning to the process for treatment;
if the concentration of the nanofiltration dialysate is more than or equal to 13 percent, performing resin separation and purification to obtain resin purified liquid;
s4, concentration and crystallization: and concentrating, crystallizing and drying the resin purified liquid to obtain a target product.
Further, in the step S2, if the concentration of the nanofiltration dialysate is between 1.0% and 13%, concentrating the dialysate, filtering the concentrated solution with a nanofiltration membrane in S2, and recovering the permeate as an eluent; if the concentration of the nanofiltration dialysate is less than 1.0%, the nanofiltration dialysate is processed to step S1 or S2 or S3 to be used as eluent.
Further, in the step S1, the primary concentrated solution is eluted and filtered by a secondary ceramic membrane to obtain a secondary concentrated solution and a secondary dialysate, the secondary dialysate is concentrated, the concentrated solution enters S2 to be filtered by a nanofiltration membrane, and the permeate is recovered as an eluent; the aperture of the secondary ceramic membrane is 50-200 nm.
Further, a nanofiltration membrane with the molecular weight cut-off less than 100 daltons is adopted in the concentration process.
Further, the resin separation and purification in the step S3 uses cation exchange and anion exchange, and the resin is continuously ion-exchanged until the conductivity is less than 100us/cm, so as to obtain the resin purified liquid.
Further, in the step S1, when the fermentation liquid is eluted through the first-stage ceramic membrane until the concentration of the first-stage concentrated solution is less than 12%, the elution is stopped; adding water into the first-stage concentrated solution through a second-stage ceramic membrane for elution until the concentration of the second-stage concentrated solution is less than 1%, and stopping elution; in step S2, the nanofiltration membrane is eluted and filtered until the concentration of the nanofiltration concentrate is less than 1%, and the elution is stopped.
Further, in the step S4, performing secondary crystallization, evaporating and concentrating the resin purified liquid in the step S3, cooling and crystallizing, and centrifuging to obtain a primary crystal and a primary mother liquid; and dissolving the primary crystal, evaporating, concentrating, cooling, crystallizing, centrifuging to obtain a secondary crystal and a secondary mother solution, and drying the secondary crystal to obtain a target product.
Further comprises the following steps of S5, mother liquor recovery: subjecting the primary mother liquor and the secondary mother liquor to chromatographic separation, decoloring and plate-frame or drum filtration to obtain a target product liquid and a residual liquid; and refluxing the target product liquid to the step S4 for crystallization and drying, and concentrating the residual liquid to be recovered as a secondary target product.
The invention also discloses an erythritol extraction system, which comprises a primary ceramic membrane filtering device, a nanofiltration membrane purifying device, a resin separation purifying device and a concentration crystallization system which are mutually connected through pipelines; the first-stage ceramic membrane filtering device comprises a first-stage concentrated solution outlet and a first-stage dialysate outlet; the primary dialysate outlet is connected with a nanofiltration membrane purification device through a pipeline; the nanofiltration membrane purification device comprises a nanofiltration concentrated solution outlet and a nanofiltration dialysate outlet; the nanofiltration dialysate outlet is provided with a grading device which can grade different outlets according to the concentration value of the nanofiltration dialysate; the grading device is provided with a plurality of grading outlets; the grading outlet is respectively connected with the resin separation and purification device and the first-stage ceramic membrane filtering device through pipelines; the resin separation and purification device is connected with the concentration and crystallization system through a pipeline.
Further, the classifying device comprises a detector for detecting the erythritol concentration and an automatic valve switch for controlling the switches of the plurality of classifying outlets.
The primary ceramic membrane filtering device comprises a primary raw material tank, a primary material conveying pump and a primary ceramic membrane separation assembly which are sequentially connected through a pipeline; the primary raw material tank is communicated with the erythritol fermentation liquor; the ceramic membrane separation aperture in the first-stage ceramic membrane separation component is 50-200 nm; a primary return pipeline is connected between the primary concentrated solution outlet and the primary raw material tank; a primary heat exchange device is arranged on the primary return pipeline, and a valve is connected between the primary raw material tank and the primary material conveying pump; the primary dialysate outlet is connected with a primary dialysis tank; the first-stage dialysis tank is connected with the nanofiltration membrane purification device through a first-stage dialysis pipeline.
The nanofiltration membrane purification device comprises a four-stage raw material tank, a four-stage material delivery pump and a nanofiltration membrane separation component which are sequentially connected through a pipeline; the four-stage raw material tank is connected with the first-stage dialysate outlet through a pipeline; the molecular weight cut-off of the nanofiltration membrane in the nanofiltration membrane separation component is 200-1000 daltons; a fourth-stage return pipeline is connected between the nanofiltration concentrated solution outlet and the fourth-stage raw material tank; four-stage heat exchange devices are installed on the four-stage return pipeline, and valves are connected between the four-stage raw material tank and the four-stage material delivery pump.
Further, the device also comprises a membrane concentration device and a two-stage ceramic membrane filtration device.
The membrane concentration device comprises a three-stage raw material tank, a three-stage material conveying pump and a concentration membrane separation assembly which are sequentially connected through a pipeline; the concentrated solution cavity of the three-stage raw material tank is connected with a nanofiltration membrane purification device through a three-stage concentration pipe; the concentration membrane separation component comprises a permeate outlet, a concentrate outlet and a nanofiltration membrane with the molecular weight cut-off less than 100 daltons; a third-stage return pipeline is connected between the concentrated solution outlet and the third-stage raw material tank; a third-stage heat exchange device is arranged on the third-stage return pipeline, and a valve is connected between the third-stage raw material tank and the third-stage material conveying pump; the permeate outlet is connected with a third-stage dialysis tank through a pipeline; the third-stage dialysis tank is connected with the first-stage ceramic membrane filtering device through a third-stage dialysis pipeline;
three grading outlets of the grading device are respectively a high-concentration grading outlet, a medium-concentration grading outlet and a low-concentration grading outlet; the high-concentration grading outlet is connected with a resin separation and purification device through a pipeline; the medium concentration grading outlet is connected with a third-stage raw material tank of the membrane concentration device; the low-concentration grading outlet is connected with the first-stage ceramic membrane filtering device;
the secondary ceramic membrane filtering device comprises a secondary raw material tank, a secondary material conveying pump and a secondary ceramic membrane separation component which are sequentially connected through a pipeline; the secondary raw material tank is connected with the primary concentration pipeline; the secondary ceramic membrane separation component comprises a secondary ceramic membrane, a secondary dialysate outlet and a secondary concentrated solution outlet, and the ceramic membrane separation aperture in the secondary ceramic membrane separation component is 50-200 nm; a second-stage return pipeline is connected between the second-stage concentrated solution outlet and the second-stage feed tank, a second-stage heat exchange device is mounted on the second-stage return pipeline, and a valve is connected between the second-stage feed tank and the second-stage feed pump; the second-stage dialysate outlet is connected with a second-stage dialysis tank through a pipeline, and the second-stage dialysis tank is connected with a third-stage raw material tank of the membrane concentration device through a second-stage dialysis pipeline;
the concentration and crystallization system comprises an evaporation concentrator, a centrifugal machine and a dryer which are connected in sequence; the evaporation concentrator is connected with a liquid outlet of the resin separation and purification device.
The invention has the advantages that:
1. the invention uses a grading device to grade nanofiltration dialysate according to the solubility, and enters different treatment procedures according to different concentrations, the nanofiltration dialysate with high concentration enters concentration crystallization, and the nanofiltration dialysate with low concentration is used as eluent for recycling. The concentration change of the system is small, the later process is stabilized, the utilization rate of the feed liquid is greatly improved, the energy consumption of subsequent evaporative crystallization is reduced, and the water consumption in the elution process is reduced.
2. The invention adopts a two-stage ceramic membrane filtering device for filtering and eluting, greatly improves the utilization rate of the feed liquid, improves the concentration of the feed liquid by using a concentration membrane concentration device, and then enters nanofiltration and filtration; the concentration change of the system is small, the later process is stable, the concentration of the feed liquid is improved, and the energy consumption of the subsequent evaporative crystallization is reduced.
3. The method uses a purification ion exchange and secondary crystallization mode to extract the erythritol, so that the accuracy of the erythritol is greatly improved.
Drawings
FIG. 1 is a process flow diagram of a first embodiment of the present invention.
FIG. 2 is a process flow diagram of a second embodiment of the present invention.
Fig. 3 is a schematic diagram of the system of the present invention.
Description of the main component symbols: 10. a first-stage ceramic membrane filtering device, 101, a first-stage raw material tank, 102, a valve, 103, a first-stage delivery pump, 104, a first-stage ceramic membrane separation component, 105, a first-stage dialysis tank, 106, a first-stage return pipeline, 107, a first-stage heat exchange device, 108, a first-stage dialysis pipeline, 109 and a first-stage concentration pipeline;
20. a secondary ceramic membrane filtering device, 201, a secondary raw material tank, 202, a valve, 203, a secondary delivery pump, 204, a secondary ceramic membrane separation component, 205, a secondary dialysis tank, 206, a secondary return pipeline, 207, a secondary heat exchange device, 208 and a secondary dialysis pipeline;
30. the device comprises a membrane concentration device, a three-stage raw material tank, a valve, a three-stage material delivery pump, a concentration membrane separation component, a three-stage dialysis tank, a three-stage reflux pipeline, a three-stage heat exchange device, a three-stage concentration pipeline, a three-stage reflux pipeline, a 307 and a three-stage heat exchange device, wherein the three-stage feed pump is 304;
40. a nanofiltration membrane purification device, 401, a four-stage raw material tank, 402, a valve, 403, a four-stage delivery pump, 404, a nanofiltration membrane separation component, 405, a four-stage return pipeline, 406, a four-stage heat exchange device, 407, a high-concentration classification outlet, 408, a medium-concentration classification outlet, 409 and a low-concentration classification outlet;
50. a resin separation and purification device, 501, a five-stage raw material tank, 502, a cation exchange column, 503 and an anion exchange column;
60. a concentration crystallization system 601, an evaporation concentrator 602, a centrifuge 603 and a dryer; 70. and (4) a grading device.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The first embodiment is as follows:
as shown in figure 1, the invention discloses an extraction process of erythritol, which comprises the following steps:
s1, ceramic membrane filtration: and eluting and filtering the erythritol fermentation liquor by a first-stage ceramic membrane to obtain a first-stage dialysate and a first-stage concentrated solution, wherein the aperture of the first-stage ceramic membrane is 50-200 nm.
S2, nanofiltration and filtration: and (5) eluting and filtering the primary dialysate obtained in the step (S1) by using a nanofiltration membrane to obtain nanofiltration dialysate and nanofiltration concentrate, wherein the molecular weight cut-off of the nanofiltration membrane is 200-1000 daltons.
S3, nano-filtration liquid classification treatment: and (3) carrying out real-time detection on the erythritol concentration of the nanofiltration dialysate in the step S2, and carrying out classification treatment:
if the concentration of the nanofiltration dialysate is less than 13%, returning to the process for treatment.
And if the concentration of the nanofiltration dialysate is more than or equal to 13 percent, performing resin separation and purification to obtain resin purified liquid.
S4, concentration and crystallization: and concentrating, crystallizing and drying the resin purified liquid to obtain a target product.
Example two:
as shown in figure 2, the invention discloses an extraction process of erythritol, which comprises the following steps:
s1, ceramic membrane filtration: filtering the fermentation liquor of erythritol (with the concentration of 15-20%, the light transmittance of more than 2%, the conductivity of less than 2000 mus/cm and the pH of 3-5) through a first-stage ceramic membrane (with the aperture of 50-200nm) to remove impurities such as mycelia in the fermentation liquor, adding water for elution, and generating a first-stage dialysate (with the concentration of 14-19%, the light transmittance of more than 2%, the conductivity of less than 2000 mus/cm and the pH of 3-5) when the solubility of the first-stage concentrated solution is less than 12%. And placing the first-stage concentrated solution in a second-stage ceramic membrane (aperture of 50-200nm) for water elution, and generating a second-stage dialysate (concentration of 1% -2%, light transmittance of more than 2%, conductivity of less than 2000 mus/cm, PH3-5) when the solubility of the second-stage concentrated solution is less than 1%. And the secondary concentrated solution is used for post treatment of waste liquid.
S2, concentration: and (3) concentrating the secondary dialysate obtained in the step S1 by using a nanofiltration membrane with the molecular weight cut-off of less than 100 daltons to obtain a concentrated solution (the refraction is more than or equal to 15%, the light transmittance is more than 2%, the conductivity is less than 2000 mus/cm, and the pH is 3-5) and a permeation solution (the refraction is 0, the light transmittance is more than 90%, and the conductivity is less than 200 mus/cm). The permeate can be recycled for elution in the second ceramic membrane in step S1 and the nanofiltration membrane in step S3.
S3, nanofiltration and filtration: and (3) eluting and filtering the primary dialysate in the step S1 and the concentrated solution in the step S2 by a nanofiltration membrane (with the molecular weight cutoff of 200 and 1000 daltons), adding water for elution in the operation process until the concentration of the nanofiltration concentrated solution is less than 1%, and generating the nanofiltration dialysate. The nanofiltration concentrated solution is used as the post treatment of waste liquid. Carrying out classification treatment on nanofiltration dialysate:
and when the concentration of the nanofiltration dialysate is more than or equal to 13%, performing resin separation and purification, namely performing cation exchange and anion exchange on the nanofiltration dialysate until the conductivity is less than 100us/cm to obtain a purified solution, thus obtaining the resin purified solution.
And when the concentration of the nanofiltration dialysate is between 1.0% and less than 13%, refluxing the nanofiltration dialysate to the nanofiltration membrane in the step S2 for concentration.
And when the concentration of the nanofiltration dialysate is less than 1.0%, the nanofiltration dialysate is recycled as eluent in the step S1 or S2 or S3.
S4, crystallizing and drying: evaporating and concentrating the purified liquid in the step S4, cooling and crystallizing, and centrifuging to obtain a primary crystal and a primary mother liquid; and dissolving the primary crystal, evaporating, concentrating and centrifuging to obtain a secondary crystal and a secondary mother solution, and drying the secondary crystal to obtain a target product. In this embodiment, the evaporation concentration is performed by using MVR, i.e., a mechanical vapor recompression technique.
S5, mother liquor recovery: performing chromatography, decoloring and plate-frame filtration on the primary mother liquor and the secondary mother liquor to obtain a target product liquor and a residual liquor; and refluxing the target product liquid to the step S4 for crystallization and drying, and concentrating the residual liquid to be recovered as a secondary target product.
Example three:
as shown in fig. 3, the present invention also discloses an extraction system of erythritol, which includes: a first-stage ceramic membrane filtering device 10, a second-stage ceramic membrane filtering device 20, a membrane concentration device 30, a nanofiltration membrane purification device 40, a resin separation purification device 50 and a concentration crystallization system 60 which are connected with each other through pipelines. The first-stage concentration pipeline 109 of the first-stage ceramic membrane filtering device 10 is connected with the second-stage ceramic membrane filtering device 20, and the second-stage dialysis pipeline 208 of the second-stage ceramic membrane filtering device 20 is connected with the membrane concentration device 30; the third-stage concentration pipeline 308 of the membrane concentration device 30 and the first-stage dialysis pipeline 108 of the first-stage ceramic membrane filtration device 10 are respectively connected with the nanofiltration membrane purification device 40; the four-stage dialysis pipeline of the nanofiltration membrane purification device 40 is provided with a classification device 70 which can classify to different outlets according to the concentration value of the nanofiltration dialysate. The classifying means 70 includes a detector for detecting erythritol concentration and an automatic valve switch for controlling the opening and closing of several classifying outlets. Three grading outlets of the grading device are arranged, namely a high-concentration grading outlet 407, a medium-concentration grading outlet 408 and a low-concentration grading outlet 409. When the concentration value of the nanofiltration dialysate detected by the detector is more than or equal to 13%, the four-stage dialysis pipeline is communicated with the high-concentration grading outlet 407 through an automatic valve switch; when the concentration value of the nanofiltration dialysate detected by the detector is between 1.0% and 13%, the four-stage dialysis pipeline is communicated with the medium concentration grading outlet 408 through an automatic valve switch; when the concentration value of the nanofiltration dialysate detected by the detector is less than 1.0 percent, the four-stage dialysis pipeline is communicated with the low-concentration grading outlet 409 through an automatic valve switch. Wherein the high concentration fractionation outlet 407 is connected to the five-stage material tank 501 of the resin separation and purification apparatus 50 through a pipe. The medium-concentration fractionation outlet 408 is connected to the tertiary feed tank 301 of the membrane concentration device 30. The low concentration fractionation outlet 409 is connected to a first-stage ceramic membrane filtration device for use as an eluent.
The first-stage ceramic membrane filtering device 10 comprises a first-stage raw material tank 101, a first-stage material conveying pump 103 and a first-stage ceramic membrane separation assembly 104 which are sequentially connected through pipelines. The primary raw material tank 101 is communicated with erythritol fermentation liquor. The ceramic membrane separation aperture in the first-stage ceramic membrane separation module 104 is 50-200 nm. The first-level ceramic membrane separation assembly 104 comprises a first-level dialysate outlet and a first-level concentrated solution outlet, a first-level return pipeline 106 is connected between the concentrated solution outlet and the first-level raw material tank 101, a first-level heat exchange device 107 is installed on the first-level return pipeline 106, and a valve 102 is connected between the first-level raw material tank 101 and the first-level delivery pump 103. The first order dislysate outlet has one-level dialysis tank 105 through the pipe connection, and one-level dialysis tank 105 is connected with the level four head tank 401 of receiving filter membrane purification device 40 through one-level dialysis pipeline 108. The concentrated solution chamber of the primary feed tank 101 is connected to the secondary feed tank 201 of the secondary ceramic membrane filtration device 20 via the primary concentrated pipe 109.
The second-stage ceramic membrane filtering device 20 comprises a second-stage raw material tank 201, a second-stage material delivery pump 203 and a second-stage ceramic membrane separation component 204 which are sequentially connected through pipelines. The ceramic membrane separation aperture in the second-stage ceramic membrane separation component 204 is 50-200nm, the second-stage ceramic membrane separation component 204 comprises a second-stage dialysate outlet and a second-stage concentrated solution outlet, a second-stage return pipeline 206 is connected between the concentrated solution outlet and the second-stage raw material tank 201, a second-stage heat exchange device 207 is installed on the second-stage return pipeline 206, and a valve 202 is connected between the second-stage raw material tank 201 and the second-stage delivery pump 203; the second-stage dialysate outlet is connected with a second-stage dialysis tank 205 through a pipeline, and the second-stage dialysis tank 205 is connected with a third-stage raw material tank 301 of the membrane concentration device 30 through a second-stage dialysis pipeline 208.
The membrane concentration device 30 comprises a three-stage raw material tank 301, a three-stage material conveying pump 303 and a concentration membrane separation assembly 304 which are sequentially connected through a pipeline. Concentrated membrane separation subassembly 304 includes permeate liquid export, concentrate export and trapped molecular weight is less than the nanofiltration membrane of 100 dalton, is connected with tertiary return line 306 between concentrate export and tertiary feed tank 301, installs tertiary heat transfer device 307 on the tertiary return line 306, is connected with valve 302 between tertiary feed tank 301 and the tertiary feeding pump 303. The permeate outlet is connected with a tertiary dialysis tank 305 through a pipeline, and the concentrated solution cavity of the tertiary raw material tank 301 is connected with a four-stage raw material tank 401 of the nanofiltration membrane purification device 40 through a tertiary concentrated pipeline 308.
The nanofiltration membrane purification device 40 comprises a four-stage raw material tank 401, a four-stage material delivery pump 403 and a nanofiltration membrane separation component 404 which are sequentially connected through pipelines. The molecular weight cutoff of the nanofiltration membrane in the nanofiltration membrane separation component 404 is 200-1000 dalton, the nanofiltration membrane separation component 404 comprises a nanofiltration dialysate outlet and a nanofiltration concentrate outlet, a four-stage return pipeline 405 is connected between the concentrate outlet and the four-stage raw material tank 401, a four-stage heat exchange device 406 is installed on the four-stage return pipeline 405, and a valve 102 is connected between the four-stage raw material tank 401 and the four-stage feed pump 403.
The resin separation and purification device 50 comprises a five-stage raw material tank 501, a cation exchange column 502 and an anion exchange column 503 which are connected in sequence.
The concentration and crystallization system 60 comprises an evaporation concentrator 601, a centrifuge 602 and a dryer 603 which are connected in sequence.
In conclusion, the invention adopts the grading device to grade the nanofiltration dialysate according to the solubility, and enters different treatment procedures according to different concentrations, thereby not only ensuring that the concentration change of the system is small and the later process is stabilized, but also greatly improving the utilization rate of the feed liquid, reducing the energy consumption of the subsequent evaporative crystallization, and simultaneously reducing the water consumption in the elution process.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention shall be covered by the scope of the present invention.
Claims (10)
1. An extraction process of erythritol is characterized in that: the method comprises the following steps:
s1, ceramic membrane filtration: eluting and filtering erythritol fermentation liquor through a first-stage ceramic membrane to obtain a first-stage dialysate and a first-stage concentrated solution, wherein the aperture of the first-stage ceramic membrane is 50-200 nm;
s2, nanofiltration and filtration: eluting and filtering the primary dialysate obtained in the step S1 by a nanofiltration membrane to obtain nanofiltration dialysate and nanofiltration concentrate, wherein the molecular weight cut-off of the nanofiltration membrane is 200 and 1000 daltons;
s3, nano-filtration liquid classification treatment: and (3) carrying out real-time detection on the erythritol concentration of the nanofiltration dialysate in the step S2, and carrying out classification treatment:
if the concentration of the nanofiltration dialysate is less than 13%, returning to the process for treatment;
if the concentration of the nanofiltration dialysate is more than or equal to 13 percent, performing resin separation and purification to obtain resin purified liquid;
s4, concentration and crystallization: and concentrating, crystallizing and drying the resin purified liquid to obtain a target product.
2. The extraction process of erythritol according to claim 1, wherein: in the step S2, if the concentration of the nanofiltration dialysate is between 1.0% and 13%, concentrating the dialysate, filtering the concentrated solution with a nanofiltration membrane in S2, and recovering the permeate as eluent; if the concentration of the nanofiltration dialysate is less than 1.0%, the nanofiltration dialysate is processed to step S1 or S2 or S3 to be used as eluent.
3. The extraction process of erythritol according to claim 1, wherein: in the step S1, the primary concentrated solution is eluted and filtered through a secondary ceramic membrane to obtain a secondary concentrated solution and a secondary dialysate, the secondary dialysate is concentrated, the concentrated solution enters S2 to be filtered through a nanofiltration membrane, and the permeate is recovered as an eluent; the aperture of the secondary ceramic membrane is 50-200 nm.
4. The extraction process of erythritol according to claim 2 or 3, wherein: and a nanofiltration membrane with the molecular weight cut-off less than 100 daltons is adopted for concentration in the concentration process.
5. The extraction process of erythritol according to claim 1, wherein: and the resin in the step S3 is separated and purified by cation exchange and anion exchange, and is continuously ion-exchanged until the conductivity is less than 100us/cm, so that resin purified liquid is obtained.
6. The extraction process of erythritol according to claim 3, wherein: in the step S1, when the fermentation liquor is eluted by the primary ceramic membrane until the concentration of the primary concentrated solution is less than 12%, the elution is stopped; adding water into the first-stage concentrated solution through a second-stage ceramic membrane for elution until the concentration of the second-stage concentrated solution is less than 1%, and stopping elution; in step S2, the nanofiltration membrane is eluted and filtered until the concentration of the nanofiltration concentrate is less than 1%, and the elution is stopped.
7. The extraction process of erythritol according to claim 1, wherein: performing secondary crystallization in the step S4, evaporating and concentrating the resin purified liquid in the step S3, cooling and crystallizing, and centrifuging to obtain primary crystals and primary mother liquid; dissolving the primary crystal, evaporating, concentrating, cooling, crystallizing, centrifuging to obtain secondary crystal and secondary mother liquor, and drying the secondary crystal to obtain a target product;
further comprises the following steps of S5, mother liquor recovery: subjecting the primary mother liquor and the secondary mother liquor to chromatographic separation, decoloring and plate-frame or drum filtration to obtain a target product liquid and a residual liquid; and refluxing the target product liquid to the step S4 for crystallization and drying, and concentrating the residual liquid to be recovered as a secondary target product.
8. An extraction system of erythritol is characterized in that: comprises a primary ceramic membrane filtering device, a nanofiltration membrane purifying device, a resin separating and purifying device and a concentration and crystallization system which are mutually connected through pipelines; the first-stage ceramic membrane filtering device comprises a first-stage concentrated solution outlet and a first-stage dialysate outlet; the primary dialysate outlet is connected with a nanofiltration membrane purification device through a pipeline; the nanofiltration membrane purification device comprises a nanofiltration concentrated solution outlet and a nanofiltration dialysate outlet; the nanofiltration dialysate outlet is provided with a grading device which can grade different outlets according to the concentration value of the nanofiltration dialysate; the grading device is provided with a plurality of grading outlets; the grading outlet is respectively connected with the resin separation and purification device and the first-stage ceramic membrane filtering device through pipelines; the resin separation and purification device is connected with the concentration and crystallization system through a pipeline.
9. The erythritol extraction system of claim 8, wherein: the grading device comprises a detector for detecting the concentration of erythritol and an automatic valve switch for controlling the switches of a plurality of grading outlets; the primary ceramic membrane filtering device comprises a primary raw material tank, a primary material conveying pump and a primary ceramic membrane separation assembly which are sequentially connected through a pipeline; the primary raw material tank is communicated with the erythritol fermentation liquor; the ceramic membrane separation aperture in the first-stage ceramic membrane separation component is 50-200 nm; a primary return pipeline is connected between the primary concentrated solution outlet and the primary raw material tank; a primary heat exchange device is arranged on the primary return pipeline, and a valve is connected between the primary raw material tank and the primary material conveying pump; the primary dialysate outlet is connected with a primary dialysis tank; the primary dialysis tank is connected with the nanofiltration membrane purification device through a primary dialysis pipeline;
the nanofiltration membrane purification device comprises a four-stage raw material tank, a four-stage material delivery pump and a nanofiltration membrane separation component which are sequentially connected through a pipeline; the four-stage raw material tank is connected with the first-stage dialysate outlet through a pipeline; the molecular weight cut-off of the nanofiltration membrane in the nanofiltration membrane separation component is 200-1000 daltons; a fourth-stage return pipeline is connected between the nanofiltration concentrated solution outlet and the fourth-stage raw material tank; four-stage heat exchange devices are installed on the four-stage return pipeline, and valves are connected between the four-stage raw material tank and the four-stage material delivery pump.
10. The erythritol extraction system of claim 9, wherein: the device also comprises a membrane concentration device and a secondary ceramic membrane filtration device;
the membrane concentration device comprises a three-stage raw material tank, a three-stage material conveying pump and a concentration membrane separation assembly which are sequentially connected through a pipeline; the concentrated solution cavity of the three-stage raw material tank is connected with a nanofiltration membrane purification device through a three-stage concentration pipe; the concentration membrane separation component comprises a permeate outlet, a concentrate outlet and a nanofiltration membrane with the molecular weight cut-off less than 100 daltons; a third-stage return pipeline is connected between the concentrated solution outlet and the third-stage raw material tank; a third-stage heat exchange device is arranged on the third-stage return pipeline, and a valve is connected between the third-stage raw material tank and the third-stage material conveying pump; the permeate outlet is connected with a third-stage dialysis tank through a pipeline; the third-stage dialysis tank is connected with the first-stage ceramic membrane filtering device through a third-stage dialysis pipeline;
three grading outlets of the grading device are respectively a high-concentration grading outlet, a medium-concentration grading outlet and a low-concentration grading outlet; the high-concentration grading outlet is connected with a resin separation and purification device through a pipeline; the medium concentration grading outlet is connected with a third-stage raw material tank of the membrane concentration device; the low-concentration grading outlet is connected with the first-stage ceramic membrane filtering device;
the secondary ceramic membrane filtering device comprises a secondary raw material tank, a secondary material conveying pump and a secondary ceramic membrane separation component which are sequentially connected through a pipeline; the secondary raw material tank is connected with the primary concentration pipeline; the secondary ceramic membrane separation component comprises a secondary ceramic membrane, a secondary dialysate outlet and a secondary concentrated solution outlet, and the ceramic membrane separation aperture in the secondary ceramic membrane separation component is 50-200 nm; a second-stage return pipeline is connected between the second-stage concentrated solution outlet and the second-stage feed tank, a second-stage heat exchange device is mounted on the second-stage return pipeline, and a valve is connected between the second-stage feed tank and the second-stage feed pump; the second-stage dialysate outlet is connected with a second-stage dialysis tank through a pipeline, and the second-stage dialysis tank is connected with a third-stage raw material tank of the membrane concentration device through a second-stage dialysis pipeline;
the concentration and crystallization system comprises an evaporation concentrator, a centrifugal machine and a dryer which are connected in sequence; the evaporation concentrator is connected with a liquid outlet of the resin separation and purification device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023066140A1 (en) * | 2021-10-19 | 2023-04-27 | 浙江华康药业股份有限公司 | Continuous membrane filtration system and filtration method for erythritol fermentation liquor |
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| CN1415631A (en) * | 2001-10-30 | 2003-05-07 | 曾和 | New technique for producing dextran |
| CN102964213A (en) * | 2012-11-23 | 2013-03-13 | 赛普特环保技术(厦门)有限公司 | Method for recovering erythritol from erythritol crystallization mother liquor |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415631A (en) * | 2001-10-30 | 2003-05-07 | 曾和 | New technique for producing dextran |
| CN102964213A (en) * | 2012-11-23 | 2013-03-13 | 赛普特环保技术(厦门)有限公司 | Method for recovering erythritol from erythritol crystallization mother liquor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023066140A1 (en) * | 2021-10-19 | 2023-04-27 | 浙江华康药业股份有限公司 | Continuous membrane filtration system and filtration method for erythritol fermentation liquor |
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