CN101560142B - Separating and refining method of arabitol in fermentation liquor - Google Patents
Separating and refining method of arabitol in fermentation liquor Download PDFInfo
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- CN101560142B CN101560142B CN2009100154545A CN200910015454A CN101560142B CN 101560142 B CN101560142 B CN 101560142B CN 2009100154545 A CN2009100154545 A CN 2009100154545A CN 200910015454 A CN200910015454 A CN 200910015454A CN 101560142 B CN101560142 B CN 101560142B
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Abstract
The invention discloses a separating and refining method of arabitol in fermentation liquor, belonging to the field of arabitol preparation. The preparation method comprises the steps of heat treatment, decolorization, ultrafiltration, chromatographic resolution and final crystallization and drying. The method improves the yield and purity of the arabitol product. Byproducts are dehydrated and concentrated to obtain crude glycerine and the yield of glycerine of the byproducts is increased, thereby increasing the economic benefits.
Description
Technical field
The present invention relates to the arabitol preparation field, arabitol separates and process for purification in specifically a kind of fermented liquid.
Background technology
The D-arabitol is of many uses, can be used as stablizer and many pharmaceutical intermediates etc. of activator, the developing material of sweeting agent, foodstuff additive, foam material.Glycerine also is a kind of important chemical material and foodstuff additive.Can be used on the chemical industry making trinitrin or Synolac etc., can be used as sweeting agent and wetting Agent for Printing Inks etc. in the food-processing industry.
The pure and mild glycerine of pectinose can be through the method preparation of biological fermentation, because the biological metabolism approach is similar, two kinds of materials often appear at in a kind of fermented liquid, and is a kind of as alternative by product appearance.Can prepare D-arabitol (H.Wouter Wisselink etc., 2007) through saccharomycetes to make fermentation D-glucose, transformation efficiency can reach 50%-60%, but the fermented liquid complicated component brings difficulty to subsequent disposal.Especially, in the by product, glycerine occupies very big ratio, has increased the decolouring of fermented liquid, concentrated difficulty.In addition, extract the method that glycerine all is the underpressure distillation of employing in traditional fermented liquid, the glycerine yield has only 60%, and purity is low, and pigment is removed difficulty, and subsequent handling is complicated.
Summary of the invention
Technical assignment of the present invention provides arabitol separation and process for purification in a kind of fermented liquid.
Technical assignment of the present invention realizes that by following mode this preparing method's step is following:
A, thermal treatment: fermented liquid poured in 4500-6000 rev/min the whizzer centrifugal 10-20 minute, and removed thalline, afterwards supernatant is heated to more than 90 ℃, be incubated 10-30 minute, regulate the pH value and be 2-4, subsequent use;
B, decolouring: add the gac of dry biomass 1%-5% in the fermented liquid after above-mentioned processing, stir, be heated to 75 ℃-90 ℃, be incubated 1-3 hour, vacuum filtration is removed gac;
C, ultrafiltration: with after the above-mentioned processing fermented liquid be 7000 ultra-filtration membrane ultrafiltration through molecular weight cut-off, further clarification;
D, chromatographic separation: 75 ℃ of temperature, adopt rotatory evaporator to be concentrated into refractive power 20%-70% the fermented liquid of above processing, in simulation moving-bed equipment, fill calcium type chromatographic separation resin; The resin total amount is 10 liters, and control condition is: input concentration is 20%-70%, flow velocity be the 0.8-3.0 liter/hour; The flow velocity that advances eluting water be the 1.0-5 liter/hour; Circulation velocity be the 4.0-9.0 liter/hour, separation temperature is 45-85 ℃, valve position switching time is 200-500 second; The flow velocity of controlling out the separation finished fluid be the 0.5-2.0 liter/hour, the flow velocity that goes out to separate sub product be the 0.8-3.0 liter/hour;
E, crystallization oven dry: with the finished fluid that obtains utilize vaporizer be concentrated into refractive power for 70%-85% about, insulation is 2-4 hour in 70-85 ℃ water-bath, is cooled to 65-75 ℃ naturally; 1-5% by solids content adds the arabitol crystal seed; Be cooled to 60-70 ℃ with 1 ℃/hour speed, be incubated 3-4 hour, be cooled to room temperature naturally; Centrifugal, get final product 45-60 ℃ of oven dry.
Fermented liquid through the control condition of ultra-filtration membrane is among the step c: input speed 0.5-3 liter/minute, pressure 0.1-0.4 kilogram.
The finished fluid of collecting in the steps d, dry substance concentration are 15%-50%, and the purity of arabitol is at 95%-99%; Sub product liquid, dry substance concentration are 10%-30%, and the purity of glycerine reaches 93%-97%.
Arabitol separates and process for purification in the fermented liquid of the present invention; Solved traditional arabitol fermentation liquor treatment difficulty, purification process is loaded down with trivial details, and yield is low; Weak points such as purity is low; Improved the yield and the purity of arabitol product, separated the purity that obtains arabitol and can reach more than 95%, can reach more than 99% through crystallization.Sub product concentrates through dewatering and obtains raw glycerine, has increased the yield of sub product glycerine, thereby has increased economic benefit.
Embodiment
Embodiment 1: get 30 liters of the fermented liquids that contains the D-arabitol that yeast fermentation D-glucose obtains, in 4500 rev/mins whizzer centrifugal 10 minutes, remove thalline and obtain the not fermented liquid of mycetome, solids content 7%; PH value 4.5 is heated to this fermented liquid more than 90 ℃, is incubated 10 minutes, regulates pH value to 2; Press 1% of amount of dry matter and add gac, stir, be heated to 75 ℃; Be incubated 1 hour, vacuum filtration is removed gac; Is 7000 ultra-filtration membrane ultrafiltration with the fermented liquid after the decolouring through molecular weight cut-off, 0.5 liter/minute of input speed, 0.1 kilogram of pressure, further clarification; At 75 ℃, adopt rotatory evaporator to be concentrated into refractive power 20% fermented liquid of above processing, high-performance liquid chromatogram determination, arabitol purity is 75%, glycerine purity is 23%.In simulation moving-bed equipment, fill calcium type chromatographic separation resin then, the resin total amount is 10 liters, and the control separation temperature is 45 ℃; Input concentration is 20%, and flow velocity is 0.8 liter/hour, and the flow velocity that advances eluting water is 1 liter/hour; Circulation velocity is 4 liters/hour; Valve position switching time is 200 seconds, and the flow velocity of controlling out separation finished fluid (main ingredient is an arabitol) is 0.5 liter/hour, and the flow velocity that goes out to separate sub product (main ingredient is a glycerine) is 0.8 liter/hour.After treatment, the finished fluid of collection, dry substance concentration are 15%, and the purity of arabitol is 95%, and sub product liquid, dry substance concentration are 10%, and the purity of glycerine is 93%.With the finished fluid that obtains, utilizing vaporizer to be concentrated into refractive power is about 70%, and insulation is 2 hours in 70 ℃ water-bath; Naturally be cooled to 65 ℃, add the arabitol crystal seed, be cooled to 60 ℃ with 1 ℃/hour speed by 1% of solids content; Be incubated 3 hours; Naturally be cooled to room temperature, centrifugal in 3000 rev/mins whizzer, 45 ℃ of oven dry.Obtain 1450 gram arabitols at last, purity is 99%, and yield is 92%.With the sub product liquid that obtains, dehydration by evaporation concentrates, and obtains raw glycerine 1.4L, and purity is 95%.
Embodiment 2: get 30 liters of the fermented liquids that contains the D-arabitol that yeast fermentation D-glucose obtains, in 6000 rev/mins whizzer centrifugal 20 minutes, remove thalline and obtain the not fermented liquid of mycetome, solids content 7%; PH value 4.5 is heated to this fermented liquid more than 90 ℃, is incubated 30 minutes, regulates pH value to 4; Press 5% of amount of dry matter and add gac, stir, be heated to 90 ℃; Be incubated 3 hours, vacuum filtration is removed gac; Is 7000 ultra-filtration membrane ultrafiltration with the fermented liquid after the decolouring through molecular weight cut-off, 3 liters/minute of input speeds, 0.4 kilogram of pressure, further clarification; At 75 ℃, adopt rotatory evaporator to be concentrated into refractive power 70% fermented liquid of above processing, high-performance liquid chromatogram determination, arabitol purity is 75%, glycerine purity is 23%.In simulation moving-bed equipment, fill calcium type chromatographic separation resin then, the resin total amount is 10 liters, and the control separation temperature is 85 ℃; Input concentration is 70%, and flow velocity is 3 liters/hour, and the flow velocity that advances eluting water is 5 liters/hour; Circulation velocity is 9 liters/hour; Valve position switching time is 500 seconds, and the flow velocity of controlling out separation finished fluid (main ingredient is an arabitol) is 2 liters/hour, and the flow velocity that goes out to separate sub product (main ingredient is a glycerine) is 3 liters/hour.After treatment, the finished fluid of collection, dry substance concentration are 50%, and the purity of arabitol is 99%, and sub product liquid, dry substance concentration are 30%, and the purity of glycerine is 97%.With the finished fluid that obtains, utilizing vaporizer to be concentrated into refractive power is about 85%, and insulation is 4 hours in 85 ℃ water-bath; Naturally be cooled to 75 ℃, add the arabitol crystal seed, be cooled to 70 ℃ with 1 ℃/hour speed by 5% of solids content; Be incubated 4 hours; Naturally be cooled to room temperature, centrifugal in 3000 rev/mins whizzer, 60 ℃ of oven dry.Obtain 1460 gram arabitols at last, purity is 99.12%, and yield is 92.6%.With the sub product liquid that obtains, dehydration by evaporation concentrates, and obtains raw glycerine 1.6L, and purity is 95.5%.
Embodiment 3: get 30 liters of the fermented liquids that contains the D-arabitol that yeast fermentation D-glucose obtains, in 5000 rev/mins whizzer centrifugal 15 minutes, remove thalline and obtain the not fermented liquid of mycetome, solids content 7%; PH value 4.5 is heated to this fermented liquid more than 90 ℃, is incubated 20 minutes, regulates pH value to 3; Press 3% of amount of dry matter and add gac, stir, be heated to 80 ℃; Be incubated 2 hours, vacuum filtration is removed gac; Is 7000 ultra-filtration membrane ultrafiltration with the fermented liquid after the decolouring through molecular weight cut-off, 2 liters/minute of input speeds, 0.25 kilogram of pressure, further clarification; At 75 ℃, adopt rotatory evaporator to be concentrated into refractive power 45% fermented liquid of above processing, high-performance liquid chromatogram determination, arabitol purity is 75%, glycerine purity is 23%.In simulation moving-bed equipment, fill calcium type chromatographic separation resin then, the resin total amount is 10 liters, and the control separation temperature is 65 ℃; Input concentration is 45%, and flow velocity is 1.5 liters/hour, and the flow velocity that advances eluting water is 3 liters/hour; Circulation velocity is 6.5 liters/hour; Valve position switching time is 350 seconds, and the flow velocity of controlling out separation finished fluid (main ingredient is an arabitol) is 1 liter/hour, and the flow velocity that goes out to separate sub product (main ingredient is a glycerine) is 2 liters/hour.After treatment, the finished fluid of collection, dry substance concentration are 30%, and the purity of arabitol is 97%, and sub product liquid, dry substance concentration are 20%, and the purity of glycerine is 95%.With the finished fluid that obtains, utilizing vaporizer to be concentrated into refractive power is about 80%, and insulation is 3 hours in 80 ℃ water-bath; Naturally be cooled to 70 ℃, add the arabitol crystal seed, be cooled to 65 ℃ with 1 ℃/hour speed by 3% of solids content; Be incubated 3.5 hours; Naturally be cooled to room temperature, centrifugal in 3000 rev/mins whizzer, 50 ℃ of oven dry.Obtain 1458 gram arabitols at last, purity is 99.1%, and yield is 92.57%.With the sub product liquid that obtains, dehydration by evaporation concentrates, and obtains raw glycerine 1.5L, and purity is 95.3%.
Claims (3)
1. arabitol separates and process for purification in the fermented liquid, it is characterized in that this preparing method's step is following:
A, thermal treatment: the fermented liquid that contains the D-arabitol that yeast fermentation D-glucose is obtained was poured in 4500-6000 rev/min the whizzer centrifugal 10-20 minute; Remove thalline, afterwards supernatant is heated to more than 90 ℃, be incubated 10-30 minute; Regulate the pH value and be 2-4, subsequent use;
B, decolouring: add the gac of dry biomass 1%-5% in the fermented liquid after above-mentioned processing, stir, be heated to 75 ℃-90 ℃, be incubated 1-3 hour, vacuum filtration is removed gac;
C, ultrafiltration: with after the above-mentioned processing fermented liquid be 7000 ultra-filtration membrane ultrafiltration through molecular weight cut-off, further clarification;
D, chromatographic separation: 75 ℃ of temperature, adopt rotatory evaporator to be concentrated into refractive power 20%-70% the fermented liquid of above processing, in simulation moving-bed equipment, fill calcium type chromatographic separation resin; The resin total amount is 10 liters, and control condition is: input concentration is 20%-70%, flow velocity be the 0.8-3.0 liter/hour; The flow velocity that advances eluting water be the 1.0-5 liter/hour; Circulation velocity be the 4.0-9.0 liter/hour, separation temperature is 45-85 ℃, valve position switching time is 200-500 second; The flow velocity of controlling out the separation finished fluid be the 0.5-2.0 liter/hour, the flow velocity that goes out to separate sub product be the 0.8-3.0 liter/hour;
E, crystallization oven dry: with the finished fluid that obtains utilize vaporizer be concentrated into refractive power for 70%-85% about, insulation is 2-4 hour in 70-85 ℃ water-bath, is cooled to 65-75 ℃ naturally; 1-5% by solids content adds the arabitol crystal seed; Be cooled to 60-70 ℃ with 1 ℃/hour speed, be incubated 3-4 hour, be cooled to room temperature naturally; Centrifugal, get final product 45-60 ℃ of oven dry.
2. arabitol separates and process for purification in the fermented liquid according to claim 1, it is characterized in that the control condition of fermented liquid process ultra-filtration membrane among the step c is: input speed 0.5-3 liter/minute, pressure 0.1-0.4 kilogram.
3. arabitol separates and process for purification in the fermented liquid according to claim 1, it is characterized in that the finished fluid collected in the steps d, and dry substance concentration is 15%-50%, and the purity of arabitol is at 95%-99%; Sub product liquid, dry substance concentration are 10%-30%, and the purity of glycerine reaches 93%-97%.
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| CN2009100154545A CN101560142B (en) | 2009-05-25 | 2009-05-25 | Separating and refining method of arabitol in fermentation liquor |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148597A (en) * | 1995-07-15 | 1997-04-30 | 塞里斯塔控股有限公司 | Method for preparation of xylitol |
| CN1284564A (en) * | 1999-06-24 | 2001-02-21 | 味之素株式会社 | Method for production of D-arabitol, D-xyloketose and xylitol |
| CN1286306A (en) * | 1999-09-01 | 2001-03-07 | 中国科学院微生物研究所 | Process for preparing arabitol by transforming glucose with yeast cells |
| CN1699587A (en) * | 2005-06-02 | 2005-11-23 | 江南大学 | Process for extracting xylose and xylitol from a xylose mother liquor or a xylose digest |
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2009
- 2009-05-25 CN CN2009100154545A patent/CN101560142B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148597A (en) * | 1995-07-15 | 1997-04-30 | 塞里斯塔控股有限公司 | Method for preparation of xylitol |
| CN1284564A (en) * | 1999-06-24 | 2001-02-21 | 味之素株式会社 | Method for production of D-arabitol, D-xyloketose and xylitol |
| CN1286306A (en) * | 1999-09-01 | 2001-03-07 | 中国科学院微生物研究所 | Process for preparing arabitol by transforming glucose with yeast cells |
| CN1699587A (en) * | 2005-06-02 | 2005-11-23 | 江南大学 | Process for extracting xylose and xylitol from a xylose mother liquor or a xylose digest |
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