CN101538589A - New clean method for producing xylitol and arabinose - Google Patents

New clean method for producing xylitol and arabinose Download PDF

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CN101538589A
CN101538589A CN200910136551A CN200910136551A CN101538589A CN 101538589 A CN101538589 A CN 101538589A CN 200910136551 A CN200910136551 A CN 200910136551A CN 200910136551 A CN200910136551 A CN 200910136551A CN 101538589 A CN101538589 A CN 101538589A
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xylitol
pectinose
temperature
fermentation
xylose mother
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张兰波
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Abstract

The invention discloses a new clean method for producing xylitol and arabinose; the method originally utilizes xylose mother liquor as raw material, improves the fermentation process and the separation and purification process by pretreatment of the xylose mother liquor, fermentation, separation of fermented fluid thalli, fermentation pre-treatment, nanofiltration, concentration, chromatographic separation of a simulated moving bed, concentration and crystallization, and the like, shortens the fermentation time, lowers the production cost, greatly reduces the discharge amount of sewage, and increases the conversion rate of xylitol and the yield rate of arabinose; the purity of the xylitol and the arabinose which are obtained by utilizing the method can respectively reach more than 99.9 percent and 99 percent; and the yield rate of xylitol and arabinose is improved greatly, thereby creating an effective clean pollution-free industrial road for the production of xylitol and arabinose.

Description

The method of a kind of novel cleaner production Xylitol and pectinose
Technical field
The invention discloses the method for a kind of novel cleaner production Xylitol and pectinose, initiated and utilized xylose mother liquid, by pre-treatment, fermentation, ceramic membrane filter, ultrafiltration, nanofiltration, simulated moving bed chromatography separation, the condensing crystal bake drying of xylose mother liquid as starting material.By improving zymotechnique and process for separating and purifying, shortened fermentation time, reduced production cost, significantly reduce the sewage emissions amount, strengthened the yield of the transformation efficiency and the pectinose of Xylitol, the xylitol purity that utilizes the inventive method to obtain can reach more than 99.9%, and pectinose can reach 99%, the yield of Xylitol and pectinose is greatly improved, and has started the industrialization road of an effective cleanliness without any pollution for the production of Xylitol and pectinose.
Technical background
Xylitol and pectinose all are polyvalent alcohols, are very important rare function sugar.Xylitol belongs to polyvalent alcohol, is a kind of novel sweetener..Edible Xylitol is difficult for producing carious tooth, and can not increase blood sugar yet, thereby be widely used in food service industry as sweeting agent, and as the clinical nutrition agent and the therapeutical agent of diabetes and hepatitis.It still is an important chemical material in addition, is widely used in aspects such as national defence, leather, plastics, coating.L-arabinose belongs to five-carbon ring aldehydo sugar, is important medicine intermediate, is mainly used to medicine synthetic anticancer, antiviral and the treatment cardiovascular disorder, also can be used as biochemical reagents, is used for the preparation of bacteria culture medium, or carries out spices and synthesize.L-arabinose also increases the reaction of carbon chain lengths with prussiate or Nitromethane 99Min., further cancellation nitrogen can generate L-glucose and L-seminose, thereby obtains how useful derivative.As long as in common sucrose, add 2% L-arabinose, just can suppress the absorption of 40% sucrose, also suppress blood glucose value simultaneously and raise about 50% less; If the L-arabinose addition reaches 4%, blood glucose value is not raise fully, Regular Insulin is secreted hardly.L-arabinose is listed in the heath food additive by U.S. food Drug Administration and Japanese health ministry approval as a kind of sweeting agent low in calories.And China has 4,000 ten thousand above diabeticss at present at least, has become the world the third-largest state of diabetes population, and the commercial value that other has 6,000 ten thousand pre-diabetes (sugar tolerance is impaired) crowds wherein to contain is also startling.But this rare function sugar price with magical function allows prestige all the time and steps back.Because separate, the restriction of purification technique, the holding at high price of L-arabinose, Japan and American-European sale price of market are 100,000-120,000 dollars/ton.And Xylitol is mainly taken from the industrial production that the hydrolysate of half fiber of plant carries out chemical reduction at present, adopt the method for pure chemistry hydrogenation as white birch, corn cob etc., not only cause product separation and purifying very difficult, and the output and the rate of recovery of Xylitol are low, high-temperature high-voltage reaction and soda acid use in a large number in the Xylitol production process, not only power consumption is big, and the production cost height has brought the risk of safety and environmental pollution simultaneously.
U.S. Pat 4816078 has been described the hemicellulose that adopts alkaline extraction to contain arabinan respectively with US6506897 from beet pulp, adopt the method for dilute acid hydrolysis hemicellulose to obtain L-arabinose then.These methods all need through hydrolysis, and the temperature of hydrolysis is than higher, damage ratio to environment is bigger, the monose that also has other L-arabinose that owing to dissociating except hydrolysis, adopt the chromatographic separation difficulty big, need L-arabinose and other monose to be separated through a few step chromatographic separation, the production cost height, level of automation is not high.
English Patent GB2408262 also is a method of extracting L-arabinose from beet pulp, requirement height to alkaline extraction, if control is improper, except arabinan was extracted, araboxylan and arabogalactan also can be extracted the purity that L-arabinose is separated in the follow-up acid hydrolysis of influence.
The aforesaid method power consumption is big, pollutes greatly, is not suitable for large-scale industrial production.
The application Chinese invention patent CN01800804.6 of Japan Unitika Ltd. has announced a kind of method that adopts enzyme to handle arabinan, Arab-xylan and Arab-Polygalactan, but this method exists the shortcoming of the inefficiency of the cost height of enzyme and enzymic hydrolysis, the later separation purification ratio is difficulty, is difficult to suitability for industrialized production.
Chinese patent CN101372700 has described a kind of method of extracting L-arabinose from xylose mother liquid and biomass acid hydrolysis liquid, mainly utilize in Dbaly yeast bacterium xylose-fermenting mother liquor or the hydrolyzed solution and cultivate, remove impurity elimination sugar, but the difficult control of fermenting process, the polyvalent alcohol that produces in the metabolic process is not explanation also, pectinose also can be utilized, and the yield that obtains pectinose is not high, only is about 33%.Utilize dehydrated alcohol to carry out pectinose and carry out crystallization, the cost height, the operability of fermentation is not very strong, a large amount of wood sugars is consumed in vain simultaneously, because need can produce a large amount of waste water through ion-exchange and decolorizing with activated carbon, pollution problem still is not resolved.
Chinese patent CN101367844 utilizes the simulated moving bed chromatography technology to extract pectinose from the gum arabic hydrolyzed solution, pectinose obtains separating with other assorted sugar such as semi-lactosi, glucuronic acids, but utilize the gum arabic hydrolysis, can pollute on the one hand, the gum arabic price comparison is expensive on the other hand, as the raw material production pectinose, can cause production cost to improve.
China Patent No. CN1107117C proposes to utilize in the production stage of various milling plants and starch plants the pars fibrosa that is obtained by plant that obtains as by product as raw material, mainly be to produce pectinose, do not relate to any purifying technique by the chaff of dilute acid hydrolysis corn grain shell (corn bran), corn ears and stems and corresponding plants.The yield of product is not high, and technology is immature, and cost is equally very high.
China Patent No. CN02116353.7 document relates to a kind of method of process for extracting L-arabinose from acacia gum by two-column.It is raw material with the gum arabic, use mineral acid hydrolysis, alkali neutralization, alcohol extraction, filter the gained resistates at last, remove insolubles through the acid dissolving, obtain the mixture of thick L-arabinose, mixture separates the mixture of pure rhamnosyl, L-arabinose and semi-lactosi through first post, the latter separates pure L-arabinose through second post, this method is owing to gum arabic price comparison height, and the height of cost recovery simultaneously causes production cost also than higher.
The raw material that China Patent No. CN101100685A produces also is to utilize the processing of corn shell (corn bran) by enzyme, dilute acid hydrolysis then, and fermentation removes assorted monose; Utilize the dehydrated alcohol crystallization to produce pectinose at last, do not relate to the production of other products.The yield of pectinose product only is 12%, and the production cost height does not conform to equally and is suitable for suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of method that is suitable for large-scale industrial production Xylitol and pectinose.
The method of a kind of novel cleaner production Xylitol and pectinose comprises the steps:
(1) activation of original strain
Original strain is inoculated in the inclined-plane solid enrichment medium, and the temperature of cultivation is 28 ℃-32 ℃, and incubation time is 72 hours-96 hours;
(2) strain expanded culture
The bacterial classification inoculation that activation is good is cultivated on the liquid enrichment medium, and culture temperature is 28 ℃-32 ℃, and oscillation number is 150-220 time/minute, and incubation time is 24 hours;
(3) the bacterial classification one grade fermemtation is cultivated
The good seed of bottle shaking culture will be shaken, inoculum size by 5%, be inoculated into 50-300 and rise in the one grade fermemtation jar, substratum is a seed culture medium, and pH value is 4.0-6.0, ventilation is 1: 0.4-0.55, jar stirs 250-350 rev/min, 28 ℃-32 ℃ of leavening temperatures, and fermentation time is 18-24 hour, do not have assorted bacterium behind the microscopy, can change the second order fermentation jar over to;
(4) the bacterial classification second order fermentation is cultivated
Fermentor tank 500-3000 liter, substratum are seed culture medium,, substratum is a seed culture medium, pH value is 4.0-6.0, and ventilation is 1: 0.4-0.55,150-230 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 20-24 hour, does not have assorted bacterium behind the microscopy, can change the three grade fermemtation jar over to;
(5) remove volatile matter in the xylose mother liquid
Xylose mother liquid is rotated evaporation, removes volatile matter in the xylose mother liquid;
(6) three grade fermemtation
Xylose mother liquid dilute with water 2-4 doubly adds nutrition composition, carries out sterilising treatment, sterilising temp is 110 ℃-115 ℃, and the time is 30 minutes, behind the bacterium of having gone out, the second class inoculum that ferments is inoculated in the three grade fermemtation jar, and tankage is the 5000-30000 liter, substratum is a fermention medium, pH value is 4.0-6.0, and ventilation is 1: between the 0.1-0.43, and 40-210 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 24-96 hour;
(7) ceramic membrane filter
The molecular weight 10000-1000000D that dams of ceramic membrane filter, the pressure of ceramic membrane filter operation is 0.4-2.0MPa, service temperature is 30 ℃-80 ℃, cycles of concentration 10-20;
(8) ultrafiltration
The molecular weight 4000-5000D that dams of ultrafiltration membrance filter, working pressure is 0.2-4MPa, and temperature is 20 ℃-55 ℃, and cycles of concentration 10-35 is doubly;
(9) nanofiltration
The nanofiltration separation membrane system is 150D-900D with the molecular weight that dams mainly, and selectivity is held back Xylitol and pectinose, and the nanofiltration working pressure is 0.2-3MPa, and temperature is 20 ℃-45 ℃, and cycles of concentration 10-35 doubly;
(10) sequential simulated moving bed chromatographic separation
Utilize calcium type or plumbous type strong acidic ion resin as separating agent, separation temperature is 60 ℃-90 ℃, and the content of the Xylitol that obtains is 8%-20%, and xylitol purity is more than 95%, and pectinose purity is more than 95%;
(11) evaporation concentration
With plate-type evaporator or falling-film evaporator, quadruple effect, vacuum tightness 0.5-0.9MPa, temperature is at 60 ℃-85 ℃, and solid content is 80%-95% when concentrating discharging;
(12) crystallization
Good Xylitol and pectinose material will be concentrated, put into crystallizer respectively, cool to 72 ℃, when whole temperature of charge uniformity, add crystal seed according to the 0.1%-10% of liquid glucose gross weight, after growing the grain 8-14 hour, begin cooling, cooling rate is 1 ℃/hour, when temperature drops to 30 ℃, crystallization finishes, and obtains xylitol crystal and pectinose crystal;
(13) dry oven dry
Start the fluidized drying bed system, heating and separating discharging in advance, xylitol crystal and pectinose crystal dropped into respectively carry out drying in the fluidized-bed, enter in the roto-sifter after the drying, Xylitol and pectinose loaf sugar are sifted out respectively, sampling analysis is dried to 0.5%, determines rank, carries out Xylitol and pectinose packing respectively;
Two, the preparation of substratum
Enrichment medium is (g/L): yeast extract paste 10, peptone 20, wood sugar 20;
Fermention medium (g/L): ammonium sulfate 0-10, potassium primary phosphate 0-5, yeast extract paste 0-5, peptone 0-4, sal epsom 0-3, xylose mother liquid 0-500;
Three, advantage of the present invention
1. do not need decolouring and ion-exchange, utilize ceramic membrane technology and nanofiltration, solved that fermented liquid concentrates, desalination, decolouring, part purification problem, labour intensity is low, the level of automation height, product is safer, purity is higher, to environment without any pollution;
2. by specific microbial strains, the waste liquid-xylose mother liquid that produces in the xylose-fermenting production process removes impurity elimination sugar, makes to separate to be more prone to, and improves the rate of recovery of Xylitol and pectinose greatly;
3. this technology has been used the simulated moving bed chromatography isolation technique, the level of automation height, and the usage quantity of having saved resin, the water yield of use is little, has improved the yield of product;
4. fermentation time and fermentation costs and traditional Xylitol and pectinose fermentation, fermentation time has shortened 50%, and xylitol yield has improved more than 30%;
5. the continuity of whole technology and level of automation height, the purifying crystal continuity in the fermentation of upstream and downstream is relatively good;
Description of drawings
Fig. 1 is the method process flow sheet of a kind of novel cleaner production Xylitol of the present invention and pectinose.
Embodiment
Embodiment 1
(1) activation of original strain
The xylitol fermentation bacterial classification that original strain adopts ATTC or Chinese microorganism strain preservation center to provide, it mainly is the candida tropicalis class, these bacterial classifications are through mutagenesis with after constantly taming, choose the energy stably express more than 20 generations, wood sugar is converted into the bacterial classification of the transformation efficiency of Xylitol at 75%-97%, original strain is inoculated in the inclined-plane solid enrichment medium, and the temperature of cultivation is 28 ℃-32 ℃, and incubation time is 72 hours-96 hours;
(2) enlarged culturing
The bacterial classification inoculation that activation is good is cultivated on enrichment medium, and culture temperature is 28 ℃-32 ℃, and oscillation number is 150-220 time/minute, and incubation time is 24 hours;
(3) one grade fermemtation is cultivated
The good seed of bottle shaking culture will be shaken, inoculum size by 5%, be inoculated in 50 liters of one grade fermemtation jars, substratum is a seed culture medium, and pH value is 4.0-6.0, ventilation is 1: 0.55, jar stirs 250-350 rev/min, 28 ℃-32 ℃ of leavening temperatures, and fermentation time is 18-24 hour, do not have assorted bacterium behind the microscopy, can change the second order fermentation jar over to;
(4) second order fermentation is cultivated
500 liters of fermentor tanks, substratum are seed culture medium,, substratum is a seed culture medium, pH value is 4.0-6.0, and ventilation is 1: 0.43,150-230 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 20-24 hour, does not have assorted bacterium behind the microscopy, can change the three grade fermemtation jar over to;
(5) remove volatile matter in the xylose mother liquid
The xylose mother liquid sugar degree is 68%-85%, ethanol about 10%.Analyze the composition that obtains sugar in the mother liquor through HPLC, wood sugar accounts for 50%, pectinose 22%, glucose 15%, semi-lactosi account for 7% and other assorted sugar, and 1 ton of xylose mother liquid is rotated evaporation, remove volatile matter in the xylose mother liquid, collect 0.1 ton of ethanol simultaneously;
(6) three grade fermemtation is cultivated
Xylose mother liquid dilute with water 2-4 doubly adds nutrition composition, carries out sterilising treatment, sterilising temp is 110 ℃-115 ℃, and the time is 30 minutes, behind the bacterium of having gone out, the second class inoculum that ferments is inoculated in the three grade fermemtation jar, and tankage is 5000 liters, substratum is a fermention medium, pH value is 4.0-6.0, and ventilation is 1: between the 0.1-0.43, and 40-210 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 24-96 hour;
(7) ceramic membrane filter
The molecular weight 30000-1000000 that dams, the pressure of ceramic membrane filter operation is 0.4-2.0MPa, service temperature is 30 ℃-80 ℃, cycles of concentration 10-20;
(8) ultrafiltration
The molecular weight 4000-5000D that dams of ultrafiltration membrance filter, working pressure is 0.2-4MPa, and temperature is 20 ℃-55 ℃, and cycles of concentration 10-35 is doubly;
(9) nanofiltration separation membrane system filtration
The molecular weight that dams is 150D-900D, and selectivity is held back Xylitol and pectinose, and the nanofiltration working pressure is 0.2-3MPa, and temperature is 20 ℃-45 ℃, and cycles of concentration 10-35 doubly;
(10) simulated moving bed chromatography is separated
Adopt sequential simulated moving bed isolation technique that Xylitol is separated with pectinose, utilize calcium type strong acidic ion resin as separating agent, separation temperature is 60 ℃-90 ℃, the content of the Xylitol that obtains is 8%-20%, xylitol purity is more than 95%, and pectinose purity is more than 95%;
(11) evaporation concentration
With plate-type evaporator or falling-film evaporator, quadruple effect, vacuum tightness 0.5-0.9MPa, temperature is at 60 ℃-85 ℃, and solid content is 80%-95% when concentrating discharging;
(12) crystallization
Good material will be concentrated, put into crystallizer, cool to 72 ℃, when whole temperature of charge uniformity, add crystal seed according to 0.1% of liquid glucose gross weight, after growing the grain 8-14 hour, begin cooling, cooling rate is 1 ℃/hour, when temperature drops to 30 ℃, crystallization finishes, and obtains 0.4 ton of xylitol crystal, 0.165 ton in pectinose crystal;
(13) dry oven dry
Start the fluidized drying bed system, heating and separating discharging in advance, xylitol crystal and pectinose crystal dropped into respectively carry out drying in the fluidized-bed, enter in the roto-sifter after the drying, Xylitol and pectinose loaf sugar are sifted out respectively, sampling analysis is dried to 0.5%, determines rank, carries out Xylitol and pectinose packing respectively;
Embodiment 2
(1) activation of original strain
The xylitol fermentation bacterial classification that original strain adopts ATTC or Chinese microorganism strain preservation center to provide, it mainly is the candida tropicalis class, these bacterial classifications are through mutagenesis with after constantly taming, choose the energy stably express more than 20 generations, wood sugar is converted into the bacterial classification of the transformation efficiency of Xylitol at 75%-97%, original strain is inoculated in the inclined-plane solid enrichment medium, and the temperature of cultivation is 28 ℃-32 ℃, and incubation time is 72 hours-96 hours;
(2) enlarged culturing
The bacterial classification inoculation that activation is good is cultivated on enrichment medium, and culture temperature is 28 ℃-32 ℃, and oscillation number is 150-220 time/minute, and incubation time is 24 hours;
(3) one grade fermemtation is cultivated
The good seed of bottle shaking culture will be shaken, inoculum size by 5%, be inoculated in 100 liters of one grade fermemtation jars, substratum is a seed culture medium, and pH value is 4.0-6.0, ventilation is 1: 0.55, jar stirs 250-350 rev/min, 28 ℃-32 ℃ of leavening temperatures, and fermentation time is 18-24 hour, do not have assorted bacterium behind the microscopy, can change the second order fermentation jar over to;
(4) second order fermentation is cultivated
1000 liters of fermentor tanks, substratum are seed culture medium,, substratum is a seed culture medium, pH value is 4.0-6.0, and ventilation is 1: 0.43,150-230 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 20-24 hour, does not have assorted bacterium behind the microscopy, can change the three grade fermemtation jar over to;
(5) remove volatile matter in the xylose mother liquid
The xylose mother liquid sugar degree is 68%-85%, methyl alcohol about 10%.Analyze the composition that obtains sugar in the mother liquor through HPLC, wood sugar accounts for 50%, pectinose 22%, glucose 15%, semi-lactosi account for 7% and other assorted sugar, and 2.2 tons of xylose mother liquids are rotated evaporation, remove volatile matter in the xylose mother liquid, collect 0.22 ton of methyl alcohol simultaneously;
(6) three grade fermemtation is cultivated
Xylose mother liquid dilute with water 2-4 doubly adds nutrition composition, carries out sterilising treatment, sterilising temp is 110 ℃-115 ℃, and the time is 30 minutes, behind the bacterium of having gone out, the second class inoculum that ferments is inoculated in the three grade fermemtation jar, and tankage is 10000 liters, substratum is a fermention medium, pH value is 4.0-6.0, and ventilation is 1: between the 0.1-0.43, and 40-210 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 24-96 hour;
(7) ceramic membrane filter
The molecular weight 30000-1000000 that dams, the pressure of ceramic membrane filter operation is 0.4-2.0MPa, service temperature is 30 ℃-80 ℃, cycles of concentration 10-20;
(8) ultrafiltration
The molecular weight 4000-5000D that dams of ultrafiltration membrance filter, working pressure is 0.2-4MPa, and temperature is 20 ℃-55 ℃, and cycles of concentration 10-35 is doubly
(9) nanofiltration separation membrane system filtration
The molecular weight that dams is 150D-900D, and selectivity is held back Xylitol and pectinose, and the nanofiltration working pressure is 0.2-3MPa, and temperature is 20 ℃-45 ℃, and cycles of concentration 10-35 doubly;
(10) simulated moving bed chromatography is separated
Adopt sequential simulated moving bed isolation technique that Xylitol is separated with pectinose, utilize calcium type strong acidic ion resin as separating agent, separation temperature is 60 ℃-90 ℃, the content of the Xylitol that obtains is 8%-20%, xylitol purity is more than 95%, and pectinose purity is more than 95%;
(11) evaporation concentration
With plate-type evaporator or falling-film evaporator, quadruple effect, vacuum tightness 0.5-0.9MPa, temperature is at 60 ℃-85 ℃, and solid content is 80%-95% when concentrating discharging;
(12) crystallization
Good material will be concentrated, put into crystallizer, cool to 72 ℃, when whole temperature of charge uniformity, add crystal seed according to 0.1% of liquid glucose gross weight, after growing the grain 8-14 hour, begin cooling, cooling rate is 1 ℃/hour, when temperature drops to 30 ℃, crystallization finishes, and obtains 0.83 ton of xylitol crystal, 0.34 ton in pectinose crystal;
(13) dry oven dry
Start the fluidized drying bed system, heating and separating discharging in advance, xylitol crystal and pectinose crystal dropped into respectively carry out drying in the fluidized-bed, enter in the roto-sifter after the drying, Xylitol and pectinose loaf sugar are sifted out respectively, sampling analysis is dried to 0.5%, determines rank, carries out Xylitol and pectinose packing respectively.

Claims (8)

1, the method for a kind of novel cleaner production Xylitol and pectinose, this method may further comprise the steps:
(1) activation of original strain
Original strain is inoculated in the inclined-plane solid enrichment medium, and the temperature of cultivation is 28 ℃-32 ℃, and incubation time is 72 hours-96 hours;
(2) strain expanded culture
The bacterial classification inoculation that activation is good is cultivated on the liquid enrichment medium, and culture temperature is 28 ℃-32 ℃, and oscillation number is 150-220 time/minute, and incubation time is 24 hours;
(3) the bacterial classification one grade fermemtation is cultivated
The good seed of bottle shaking culture will be shaken, inoculum size by 5%, be inoculated into 50-300 and rise in the one grade fermemtation jar, substratum is a seed culture medium, and pH value is 4.0-6.0, ventilation is 1: 0.4-0.55, jar stirs 250-350 rev/min, 28 ℃-32 ℃ of leavening temperatures, and fermentation time is 18-24 hour, do not have assorted bacterium behind the microscopy, can change the second order fermentation jar over to;
(4) the bacterial classification second order fermentation is cultivated
Fermentor tank 500-3000 liter, substratum are seed culture medium,, substratum is a seed culture medium, pH value is 4.0-6.0, and ventilation is 1: 0.4-0.55,150-230 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 20-24 hour, does not have assorted bacterium behind the microscopy, can change the three grade fermemtation jar over to;
(5) remove volatile matter in the xylose mother liquid
Xylose mother liquid is rotated evaporation, removes volatile matter in the xylose mother liquid;
(6) three grade fermemtation
Xylose mother liquid dilute with water 2-4 doubly adds nutrition composition, carries out sterilising treatment, sterilising temp is 110 ℃-115 ℃, and the time is 30 minutes, behind the bacterium of having gone out, the second class inoculum that ferments is inoculated in the three grade fermemtation jar, and tankage is the 5000-30000 liter, substratum is a fermention medium, pH value is 4.0-6.0, and ventilation is 1: between the 0.1-0.43, and 40-210 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 24-96 hour;
(7) ceramic membrane filter
The molecular weight 10000-1000000D that dams of ceramic membrane filter, the pressure of ceramic membrane filter operation is 0.4-2.0MPa, service temperature is 30 ℃-80 ℃, cycles of concentration 10-20;
(8) ultrafiltration
The molecular weight 4000-5000D that dams of ultrafiltration membrance filter, working pressure is 0.2-4MPa, and temperature is 20 ℃-55 ℃, and cycles of concentration 10-35 is doubly;
(9) nanofiltration
The nanofiltration separation membrane system is 150D-900D with the molecular weight that dams mainly, and selectivity is held back Xylitol and pectinose, and the nanofiltration working pressure is 0.2-3MPa, and temperature is 20 ℃-45 ℃, and cycles of concentration 10-35 doubly;
(10) sequential simulated moving bed chromatographic separation
Utilize calcium type or plumbous type strong acidic ion resin as separating agent, separation temperature is 60 ℃-90 ℃, and the content of the Xylitol that obtains is 8%-20%, and xylitol purity is more than 95%, and pectinose purity is more than 95%;
(11) evaporation concentration
With plate-type evaporator or falling-film evaporator, quadruple effect, vacuum tightness 0.5-0.9MPa, temperature is at 60 ℃-85 ℃, and solid content is 80%-95% when concentrating discharging;
(12) crystallization
Good Xylitol and pectinose material will be concentrated, put into crystallizer respectively, cool to 72 ℃, when whole temperature of charge uniformity, add crystal seed according to the 0.1%-10% of liquid glucose gross weight, after growing the grain 8-14 hour, begin cooling, cooling rate is 1 ℃/hour, when temperature drops to 30 ℃, crystallization finishes, and obtains xylitol crystal and pectinose crystal;
(13) dry oven dry
Start the fluidized drying bed system, heating and separating discharging in advance, xylitol crystal and pectinose crystal dropped into respectively carry out drying in the fluidized-bed, enter in the roto-sifter after the drying, Xylitol and pectinose loaf sugar are sifted out respectively, sampling analysis is dried to 0.5%, determines rank, carries out Xylitol and pectinose packing respectively.
2, as claim 1 bacterial classification mainly from Candida tropicalis, Candida shehatae, Candida spandovensis, Candida utilis, Candida guilliermondii, Candida fragi, Candida intermedia, SIIM Y258 Geotrichumcandidum, SIIM Y282 Geotrichum suaveolens, SIIM Y140 Geotrichum candidum Halomonas sp.MCCC 1B01019, SIIM Y276 Pachysolen tannopHilus SIIM Y340 Wickerhamia fluorescens etc., these bacterial classifications choose the energy stably express more than 20 generations through mutagenesis with after constantly taming, wood sugar is converted into the bacterial classification of the transformation efficiency of Xylitol at 75%-97%, adopts single culture or fermented by mixed bacterium.
3, the raw material as claim 1 production Xylitol and pectinose comprises: xylose mother liquid, xylose mother liquid+corn cob hydrolyzed solution, xylose mother liquid+wheat bran hydrolyzed solution, xylose mother liquid+white birch bark hydrolyzed solution, xylose mother liquid+bagasse hydrolyzed solution, xylose mother liquid+rice husk hydrolyzed solution, xylose mother liquid+cotton seed hulls hydrolyzed solution.
4, as the used condition of claim 1 fermentation
(1) enrichment medium is (g/L): yeast extract paste 10, peptone 20, wood sugar 20.Fermention medium (g/L): ammonium sulfate 0-10, potassium primary phosphate 0-5, yeast extract paste 0-5, peptone 0-4, sal epsom 0-3, xylose mother liquid 0-500;
(2) pH value is 4.0-6.0, and ventilation is 1: between the 0.1-0.43, and 40-210 rev/min of jar stirring, 28 ℃-32 ℃ of leavening temperatures, fermentation time is 24-96 hour.
5, as claim 1,2,3,4, the working condition of Xylitol and pectinose can be used in the fermentation volume of 0-30 ton.
6, comprise ceramic membrane filter, ultrafiltration, nanofiltration system as claim 1,4,5 filtering systems.The molecular weight 30000-1000000D that dams of ceramic membrane filter utilizes ceramic membrane filter to remove thalline colloidal solid remaining in the fermented liquid, protein, nucleic acid molecule, partial pigment etc.Reclaim thalline simultaneously, these thalline are used for circulating fermentation.Ultrafiltration thalline colloidal solid, protein, nucleic acid molecule, partial pigment improve the effect of nanofiltration.The nanofiltration system selective filter is removed Nucleotide, amino acid, small peptide oligose, partial pigment, the salinity in the fermented liquid wherein; Hold back the molecule of molecular weight between 150D-300D, be mainly Xylitol and pectinose.
7, adopt sequential simulated moving bed isolation technique as claim 1, pectinose and Xylitol are reclaimed.Utilize calcium type or plumbous type strong acidic ion resin as separating agent, separation temperature is 60 ℃-90 ℃, water is as eluent, and dosage of crosslinking agent is the 3%-30% of calcium type or plumbous type strong acidic ion resin weight, and linking agent is selected triethylene benzene, divinylbenzene or the rare benzene of dipropyl etc. for use.
8, as claim 1 evaporation concentration with plate-type evaporator or falling-film evaporator, quadruple effect, vacuum tightness 0.5-0.9MPa, temperature is at 60 ℃-85 ℃, solid content is 80%-95% when concentrating discharging.The crystalline method: Tc is 72 ℃, when whole temperature of charge uniformity, adds crystal seed according to the 0.1%-10% of liquid glucose gross weight, after growing the grain 8-14 hour, begins cooling, and cooling rate is 1 ℃/hour, and when temperature dropped to 30 ℃, crystallization finished.
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