CN1661027A - Process for producing fructose by using chicory for hydrolysis - Google Patents
Process for producing fructose by using chicory for hydrolysis Download PDFInfo
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- CN1661027A CN1661027A CN 200410073352 CN200410073352A CN1661027A CN 1661027 A CN1661027 A CN 1661027A CN 200410073352 CN200410073352 CN 200410073352 CN 200410073352 A CN200410073352 A CN 200410073352A CN 1661027 A CN1661027 A CN 1661027A
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- 235000007542 Cichorium intybus Nutrition 0.000 title claims abstract description 45
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 38
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 38
- 229930091371 Fructose Natural products 0.000 title claims abstract description 37
- 239000005715 Fructose Substances 0.000 title claims abstract description 36
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 25
- 241000723343 Cichorium Species 0.000 title abstract description 5
- 229920001202 Inulin Polymers 0.000 claims abstract description 85
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Abstract
The invention relates to a process for producing fructose by hydrolyzing inulin extracted from chicory, which has the advantages of simple and reasonable technical route, easy control, high production efficiency and low production cost, and can simultaneously select and obtain diversified products according to needs, such as high fructose syrup produced by acid hydrolysis, chicory sugar mixture (namely, PPE) produced by incomplete hydrolysis of inulase, fructo-oligosaccharide produced by fermentation of endo-inulase and ultrahigh fructose syrup produced by fermentation of exoinulase. The product obtained by the production process has good purity, high concentration and good quality.
Description
Technical field
The invention belongs to chemical industry and extract the field, particularly a kind ofly utilize witloof to be hydrolyzed to produce the technology of fructose.
Background technology
Fructose is a kind of form of preserving energy in the cereal, extensively has been used to foodstuffs industry recently and has made sweeting agent, because it than the sweet 1.5-1.7 of sucrose doubly, and heat content is low.Traditional mode of production fructose method is to obtain glucose by starch by acidolysis or enzymolysis, and glucose generates fructose under the effect of isomerase.Containing fructose in the fructose syrup that obtains by this technology is 42%, as seeks out high fructose syrup and then need to continue concise, and just can obtain concentration is 55% fructose, does not reach industrial required fructose standard on the one hand, and complex process, wastes raw material, and cost is higher.Therefore, produce the focus that fructose or oligofructose become the fructose industry research by acid hydrolysis or inulinase hydrolytic inulin.
Inulin by the different polymerization degree Polylevulosan form mixture, the Polylevulosan of the polymerization degree lower (polymerization degree is between 2～9) such as inulin trisaccharide, inulin tetrose, inulin pentasaccharides wherein, be commonly referred to oligofructose, all the other are made up of the Polylevulosan of the polymerization degree between 20～60 substantially.Inulin can be hydrolyzed into and be oligofructose and fructose.Oligofructose is because because low heat value and health properties have become a kind of functional food additives that is subjected to welcome both at home and abroad and approval deeply.High fructose syrup that hydrolysis of inulin generates and superelevation fructose syrup are called as the third generation glycogen after sucrose, Dian Fentang, because its high sugariness and low-calorie performance become the new lover of food service industry.In addition, witloof itself also is a kind of extraordinary herbage, wherein contained inulin is through not exclusively the ferment mixture of the witloof sugar that generates of inulinase, without any processing convection drying, the effect that domestic animal, poultry is had propagation bifidus bacillus, enhancing resistance against diseases, be a kind of very good feed additives, be called as plasmosin PPE.
At present industrial applied oligofructose, high fructose syrup and superelevation fructose syrup and witloof plasmosin PPE are that water by inulin or inulin produces.
Contain the plant of enriching inulin and mainly contain jerusalem artichoke, Garden Dahlia root and witloof etc., development abroad has nearly centenary history.Domestic the eighties begins to introduce witloof, and the nineties just begins to start to walk to carry out the research of inulin.
The Chinese patent publication number is that the patent application of CN1389468A discloses the method that direct membrane sepn is produced inulin, oligofructose, be fructose and inulin and other component separating with itself contains in the plant, and obtain purified oligofructose and fructose, the fructose of Sheng Chaning yields poorly like this, is difficult to satisfy market demand; The Chinese patent publication number is the patent of CN1288472A, mainly be the technology of producing the standard level chicory inulin that improves mean polymerisation degree, or carry out etherificate, esterification, carboxylated etc. to obtaining synanthrin, the synanthrin that obtains improveing, there are not low molecular monose, biglycan, oligose etc. in the product of producing, so so-called chicory inulin refers to the inulin of ordinary meaning here.
Summary of the invention
The object of the present invention is to provide a kind of technology of utilizing witloof to be hydrolyzed to produce fructose.
In order to realize above-mentioned task, the technical scheme that the present invention takes is, a kind ofly utilizes witloof to be hydrolyzed to produce the technology of fructose, it is characterized in that, adopt the inulin in the witloof to produce witloof plasmosin or superelevation fructose syrup or oligose or high fructose syrup, comprise the following steps:
The inulin of producing witloof plasmosin or superelevation fructose syrup or oligose extracts:
Root of Herba Cichorii crushing and water-adding after the Rapid Cleaning is soaked, 10 ℃-45 ℃ of water temperatures, the time is 20-30min; Or with the immersion of drying sheet root crushing and water-adding, 30 ℃-95 ℃ of water temperatures; Time is 20-60min, is heated to 75 ℃ of-100 ℃ of lixiviates then, and the time is 40min, carries out three adverse current lixiviates, after the washery slag operation, obtains thick aqueous extract; The inulin that is used to prepare plasmosin keeps former slag;
The inulin of producing high fructose syrup extracts:
Root of Herba Cichorii crushing and water-adding after the Rapid Cleaning is soaked, 10 ℃-45 ℃ of water temperatures, the time is 20-30min; Or with the immersion of drying sheet root crushing and water-adding, 30 ℃-95 ℃ of water temperatures; Time is 20-60min, and right using between its PH to 3.0-6.5 of acid accent under 30-75 ℃ of condition, placed 2 hours, filtered and regulate PH to 3.0-4.5 then, obtained hydrolysis material;
Then the inulin that obtains is produced qualified product according to the preparation technology of witloof plasmosin or superelevation fructose syrup or oligose or high fructose syrup.
The preparation of described witloof plasmosin is undertaken by following step:
(1) fermentation: the thick aqueous extract that will obtain, inulinase direct hydrolysis in enzyme reactor, utilize endo-inulinase to regulate fermented liquid, can obtain the oligofructose solution of complete hydrolysis or partial hydrolysis at PH 3.0-6.6, temperature 40-70 ℃, pol 25%, time 2-20 hour;
(2) enzyme that goes out: above-mentioned dreggy oligofructose solution is delivered to sterilization in the disinfection tank, and germ-resistant purpose is killed the arbitrary bacterium in the feed liquid and is made enzyme denaturation, 80 ℃～110 ℃ of Heating temperatures, time 5-15min, or select the higher temperature instantaneous sterilization, make protein coagulating, later cooling immediately;
(3) abrasive dust: the raw material behind the enzyme that will go out grinds processing, obtains pasty state solution;
(4) spraying drying: obtain pasty state solution and obtain powdery product, be the witloof plasmosin by spraying drying, forced air drying, drying bu sublimation.
The preparation of described superelevation fructose syrup or oligose is undertaken by following step:
(1) milk of lime is handled: the thick aqueous extract that is rich in inulin is cooled to 40-50 ℃, add milk of lime reagent at thick aqueous extract, and pH value transferred to 13.5, feed carbon dioxide then, protein, pectin and non-sugar colloid in the inulin crude extract are precipitated rapidly, and by filtration under diminished pressure, plate-and-frame filter press or whizzer precipitated impurities is separated with filtrate, obtain purified inulin extracting solution;
(2) enzyme that goes out is handled: the extracting solution that will be rich in inulin send and causes in the disinfection tank sterilization and make enzyme denaturation, solidifying protein, and Heating temperature is more than 90 ℃, below 110 ℃, time 5-15min, or select the higher temperature instantaneous sterilization, make protein coagulating, later cooling immediately;
(3) membrane filtration is removed thalline, water-soluble protein, pigment and other insolubles: select the aperture in 0.05-0.2 μ m or aperture the inorganic ultra-filtration membrane of tubular fibre at 0.05-0.1 μ m, remove thalline fully, solidify and water-soluble protein, colloid, pigment and other insolubles, obtain the clarifying aqueous extract that is rich in inulin;
(4) macroporous adsorbent resin decolouring: will pass through macroporous adsorbent resin through the aqueous extract that is rich in inulin of above-mentioned processing, and collect water elution liquid, and obtain inulin solution through decolouring;
(5) the electrodialysis ion-exchange membrane is handled: with the aperture is that 0.001～0.01 electrodialysis ion-exchange membrane removes inorganic, the organic ion in the inulin solution, obtains making with extra care inulin solution;
(6) to above-mentioned obtain refining inulin solution adopt endo-inulinase hydrolysis or alantin excision enzyme hydrolysis can obtain highly purified oligofructose or contain that fructose is 92%, glucose is less than 3% superelevation fructose syrup.
The preparation of described high fructose syrup is undertaken by following step:
(1) acid hydrolysis: the hydrolysis material that obtains is placed in the hydrolysis reactor, pH value between 3-6,120 ℃～160 ℃ of temperature, time 1-10min obtains hydrolysate;
(2) decolouring of high fructose syrup, desalination: hydrolysate at first ion-exchange gel chromatography removes by filter ash content, twice ion-exchange-resin process removes albumen then: earlier with strong acidic cation-exchange resin wash-out under greater than 70 ℃ condition, and then through weakly acidic cation-exchange resin, exchange by secondary ions, protein reduces 50% in the solution, dipolymer drops to 2.9% by 4.4%, and carbohydrate accounts for soluble material 12%; At last by gac formula charcoal bed depigmentation;
(3) collect solid: under the decompression situation, 50-100 ℃ concentrates, or 100-120 ℃ of normal pressure is concentrated, and the time is no more than 1 hour, and drying bu sublimation can obtain high fructose syrup then.
The condition of described endo-inulinase hydrolysis is: 42 ℃-80 ℃ of fermented liquid temperature, and the PH of solution is 5-6.5, inulenin concentration 10%-30%, enzyme effect dosage is 2-30U/g, time 6-30 hour; After the endo-inulinase hydrolysis, 90-120 ℃ acts on 1-5 minute, makes enzyme deactivation.
The condition of described alantin excision enzyme hydrolysis is: 50 ℃-65 ℃ of temperature, PH is 5-6, time is 1-5 hour, and the alantin excision enzyme of adding 0.15v/v, containing fructose in the liquid syrup that obtains is 72%, and glucose is 28%, colourless slurries, then above-mentioned slurries are concentrated to original 20%, the transparent golden yellow slurries that promptly obtain.
The membrane technique in technology utilization modern times of the present invention is wanted to combine with classical chemical process technology, give full play to advantage separately, reduce production costs, further improve the quality of products, and diversified product such as witloof sugar mixture (being witloof plasmosin PPE), oligofructose, high fructose syrup and superelevation fructose syrup are provided.
Description of drawings
Fig. 1 is processing technology routine figure of the present invention;
Fig. 2 is the production process route figure of the plasmosin PPE of embodiments of the invention 1;
Fig. 3 is the production process route figure of the oligose of embodiments of the invention 2 high densitys;
Fig. 4 is the production process route figure that embodiments of the invention 3 are produced high fructose;
Fig. 5 is the production process route figure of embodiments of the invention 4 production superelevation fructose syrups.
The embodiment that provides below in conjunction with accompanying drawing and contriver is described in further detail operational path of the present invention.
Embodiment
The production technology route of invention can be for a more detailed description to the Technology content in the production process of invention from figure referring to Fig. 1.
The present invention is the various fructose of production feedstock production with the witloof, comprises witloof plasmosin or superelevation fructose syrup or oligose or high fructose syrup.
1, raw material is handled:
At first, the fresh root of Herba Cichorii of harvesting will be excavated, Rapid Cleaning in cleaning machine, remove earth, Shi Sha and other foreign material etc., the time of soaking and washing is short as much as possible, because along with the prolongation of soak time, the sugar degree in the wash water liquid increases, the loss of sugar is big more, preferably is no more than one hour on the time; Chiccory root tuber part after the cleaning enters production, and mechanical disintegration is directly processed.
The chiccory root tuber that can't finish processing the short period of time after the cleaning, section, rapidly drying treatment is stored, perhaps the high temperature dry storage again of going out behind the enzyme.The section purpose allows big as far as possible area contact water be easy to lixiviate, notices that the thickness of section is preferably between the 0.5-1cm, and maximum is no more than 2cm, approaches excessively to be unfavorable for filtering; The content that makes water is that the original 10%-30% of raw material is advisable.Note controlled temperature during heating more than 70 ℃, when temperature rises to 50-70 ℃, skip as much as possible rapidly, prevent that inulinase is activated, cause a large amount of degradeds of inulin, cause the loss of sugar.Heating or rapidly drying can make the inulinase inactivation, make simultaneously that inulin exists with solid form in the enchylema.
For cleaning Manufactured witloof dry plate in the process of storing, can adhere to a large amount of impurity such as dust, express 2-15min, can leach a part of pigment, the loss of sugar also seldom, if the time lengthening of embathing is to 15min, although elutant color burn, can remove partial pigment, but the loss excessive (more than 10%) of sugar, so the cleaning of witloof dry plate is best with 2-10min.
2, the extraction of inulin:
(1) inulin that is used for plasmosin, superelevation fructose syrup and oligose preparation extracts: at first soak, and 10 ℃ of the water temperatures-45 ℃ (enzyme does not go out) that bright root soaks, if water temperature is high, inulinase is activated, and can cause the degraded of inulin, the time is 20-30min; It is 30-95 ℃ that the drying sheet root soaks water temperature; Time is that 20-60min gets final product.Heat lixiviate then: optimum temps is 75 ℃-100 ℃, and the time is 40min, generally carries out three adverse current lixiviates, a washery slag operation.The adverse current lixiviate can produce maximum concentration difference, and lixiviate is carried out effectively.At last, press filtration or the centrifugal crude extract that obtains being rich in inulin; The inulin that is used for the plasmosin preparation can keep former slag, and former slag is also capable of using as feed.
(2) inulin that is used for the high fructose syrup preparation extracts: bright root of pretreated witloof or witloof sheet slag soak, blend, and transfer between its PH to 3.0-6.5 with acid, under 30-75 ℃ of condition, place 2 hours, make more inulin dissolving.Preferably select to form volatile acid such as hydrogen sulfide, sulfurous gas, formic acid, carbonic acid, acetate etc.Filter and adjusting PH to 3.0-4.5, use SO
2It is best to regulate pH value, can reduce impurity.
3, witloof plasmosin PPE preparation:
(1) fermentation: the aqueous extract that is rich in inulin that the process pre-treatment obtains, inulinase direct hydrolysis in enzyme reactor utilizes any endo-inulinase to regulate the oligofructose solution that fermented liquid PH3.0-6.6, temperature 40-70 ℃, pol about 25%, time 2-20 hour can obtain complete hydrolysis or partial hydrolysis.
(2) enzyme that goes out: dreggy oligofructose is prepared liquid deliver to sterilization in the disinfection tank, germ-resistant purpose is killed the arbitrary bacterium in the feed liquid and is made enzyme denaturation, Heating temperature is more than 80 ℃, below 110 ℃, time 5-15min, also can select more high-temperature instantaneous sterilization, germ-resistant principle is the suitable high protein coagulating that extremely enough makes of temperature, pressure.For preventing the thermolysis of inulin, cooling immediately later.
(3) abrasive dust: be convenient to preserve the allotment of getting food, digestion and feed with animal in order to reduce volume, be necessary by fermentation witloof raw material is ground processing, obtain pasty state solution.
(4) spraying drying: can obtain powdery product by spraying drying, forced air drying, drying bu sublimation, promptly witloof plasmosin PPE can make functional feedstuff additive.
4, the preparation of high fructose syrup:
(1) acid hydrolysis: be placed in the hydrolysis reactor by above-mentioned 2 (2) hydrolysis material that obtain, controlled temperature is about 120-160 ℃, and time 1-10min obtains hydrolysate.Filter, obtain thick fructose extracting solution.This be reflected at pH value between the 3-6 with the condition of no enzyme under high molecular fructose become single fruit sugar by complete hydrolysis.Acid hydrolysis products contains the impurity such as carbohydrate, 8.7% salt and pigment of 1-5%, and 4.7% protein, therefore needs further desalination bleaching.
(2) decolouring of high fructose syrup, desalination
1. hydrolysate at first ion-exchange gel chromatography (DOWEX Monsophere) remove by filter ash content, 2. twice ion-exchange-resin process removes albumen then: earlier with strong acidic cation-exchange resin (as Dowex88) wash-out under greater than 70 ℃ condition, and then through weakly acidic cation-exchange resin (Dowex66), can making more, the hydrolysis of inulin of deep layer takes place.By the secondary ions exchange, protein reduces 50% in the solution, and dipolymer drops to 2.9% by 4.4%, and carbohydrate accounts for soluble material 12%, and these steamed bun stuffed with sugars are drawn together 2.9% disaccharides, 71.4% fructose, 25.7% glucose.3. by gac formula charcoal bed depigmentation.
(3) collect solid: under the decompression situation, 50-100 ℃ concentrates, or 100-120 ℃ of normal pressure is concentrated, and the time is no more than 1 hour, and drying bu sublimation obtains high fructose then.
5, inulin extracting solution refining that is used for the preparation of superelevation fructose syrup and oligose:
(1) milk of lime is handled: the inulin extracting solution is except inulin, the protein that also contains some amount, pectin, organic acid, Mierocrystalline cellulose and other composition, leach in the process of extracting inulin witloof, these impurity not only have a strong impact on the quality of inulin, and because they become colloidal state, cause the extracting liquid filtering process very difficult, also make simultaneously the desalination in the production process, decolouring and enrichment process can't carry out smoothly, therefore must carry out decon to the inulin extracting solution handles, effectively improve inulin extracting liquid filtering situation, remove the non-sugar impurity that suspended substance and removal as much as possible are dissolved in the inulin extracting solution fully, therefore the present invention adopted the milk of lime removal of impurities earlier before entering next process.
Method is after extracting solution is cooled to 40-50 ℃, add milk of lime reagent, make extracting solution reach PH=13.5, feed carbon dioxide then, non-sugar colloids such as protein in the inulin extracting solution, pectin are precipitated rapidly, and by filtration under diminished pressure, plate-and-frame filter press or whizzer precipitated impurities is separated with filtrate, obtain the inulin crude extract.
This method operation rapidly, various Impurity removals are thorough, and do not introduce the impurity of new difficult removal, filtrate after the processing meets the processing requirement of next process, for the purity requirement of the finished product provides guarantee, the cost of the carbonic acid gas that unslaked lime that this method is used and the unslaked lime of firing produce is not high yet, is very economical and practical production operation method.
(2) the inulin crude extract enzyme that goes out is handled: the extracting solution that will be rich in inulin send and causes sterilization in the disinfection tank, germ-resistant purpose is killed the arbitrary bacterium in the feed liquid and is made enzyme denaturation, solidifying protein, Heating temperature is more than 90 ℃, below 110 ℃, time 5-15min also can select more high-temperature instantaneous sterilization, and germ-resistant principle is the suitable high protein coagulating that extremely enough makes of temperature, pressure.For preventing the thermolysis of inulin, cooling immediately later.
(3) membrane filtration is removed thalline, water-soluble protein, pigment and other insolubles: preferred aperture is at 0.05-0.2 μ m, preferably select the tubular fibre inorganic ultra-filtration membrane of aperture at 0.05-0.1 μ m, remove thalline fully, solidify and water-soluble protein, colloid, pigment and other insolubles, obtain the clarifying aqueous extract that is rich in inulin.
Modern membrane technology is an aperture feature of utilizing film, separate with the molecule of physical means different sizes, sepn process is not heated, stable components, separation rate height, power consumption are low, and non-secondary pollution has very big advantage to the removal of particulate and the separation of water-soluble macromolecule.Can remove particulate, pyrogen, microorganism well as ultra-filtration membrane 6000-10000 molecular weight ultra-filtration membrane, the quality of raising preparation and stability thereof, security.But cost an arm and a leg, need protection meticulously to use.So adopt alkali lye precipitation-ultra-filtration membrane-integrated impurity removal method of centrifugation, give full play to advantage separately, reduced the pollution of film, reduced cost, improved quality.
(4) macroporous adsorbent resin decolouring: macroporous adsorbent resin is the organic polymer sorbent material that has grown up since the seventies, has absorption property preferably, is the parting material that absorption and screening combine.Its physico-chemical property is stable, is insoluble to acid, alkali and organic solvent, and is good to organic selectivity, the influence that not existed by inorganic salts and strong particle low molecular compound, and especially it is very poor to the adsorptive power of carbohydrate, and the adsorptive power of polychrom is very strong.Method is that the inulin solution through above-mentioned processing is fully dissolved, by macroporous adsorbent resin, and, impurity such as pigment are collected water elution liquid by resin absorption, obtain the inulin solution through decolouring.The optional D-101 type of macroporous adsorbent resin, DA-201 type or MD-05271 type, GDX-105 type and D-G type etc. all can.
(5) the electrodialysis ion-exchange membrane is handled: with the aperture is that 0.001～0.01 electrodialysis ion-exchange membrane removes inorganic, the organic ion in the solution, obtains making with extra care inulin solution.
Sepn process is not heated, stable components, separation rate height, power consumption are low, and non-secondary pollution is behind the inulin solution resin purification, the composition of polluted membrane is reduced greatly, and both combinations can be given full play to advantage separately, complementary the other side's deficiency more has an economic benefit than independent use film.
6, the preparation of oligofructose:
Condition during the inulinase hydrolysis: 42-80 ℃ of fermented liquid temperature, 45-70 ℃ of optimum; The PH=5-6.5 of regulator solution is slightly acidic; Inulenin concentration 10%-30%, about the best 20%, the best; Enzyme amount 2-30U/g, time 6-30 hour; After endo-inulinase (EC3.2.1.7) hydrolysis, 90-120 ℃ went out enzyme 3-15 minute, obtained highly purified oligofructose.
7, superelevation fructose syrup preparation:
Alantin excision enzyme (EC3.2.1.80) hydrolysis obtains high purity fructose.At 50 ℃-65 ℃, PH is 5-6, and the time is 1-5 hour, adds the alantin excision enzyme of 0.15v/v. obtain liquid syrup in to contain fructose be 72%, glucose is 28%, colourless slurries.Above-mentioned slurries are being concentrated to 20% original transparent golden yellow slurries that obtain.Then containing fructose in this is 92%, glucose less than 3%.
Below be that the contriver is the preferred embodiment that example provides with the witloof, wherein the extraction of inulin is all undertaken by the method for above-mentioned production witloof plasmosin or superelevation fructose syrup or oligose or high fructose syrup.
Embodiment 1: the production of plasmosin PPE
Referring to Fig. 2, undertaken by the preparation method of above-mentioned plasmosin, be that 95 ℃ hot water lixiviate is filtered with 7 kilograms of the bright root of Herba Cichorii of 10 kilograms of pulverizing or witloof dry plates in temperature, solid-liquid ratio=1: 2～3, promptly obtain being rich in the mixed solution of inulin at 30 minutes time; Regulate fermented liquid at PH4.0 with endo-inulinase then, 50 ℃ of temperature, pol 25%, 12 hours time; 105 ℃ of enzymes that go out, time 8min, through grinding, spraying drying under 100 ℃ of conditions, obtain 6.313 kilograms of isabelline extract witloof plasmosins (PPE).
Example 2: the production of high density oligose
Referring to Fig. 3, preparation method by above-mentioned oligose carries out, bright root of 10 kilograms of witloofs or witloof dry plate are that 95 ℃ hot water lixiviate is filtered in temperature, through three adverse current lixiviates, obtain the inulin crude extract after one time the washery slag operation is handled, the inulin crude extract that obtains is cooled to 45 ℃, through 90 ℃ of sterilizations and the removal of impurities of adding milk of lime, transfer PH=13.5, feed carbonic acid gas, remove unnecessary calcium ion, and precipitated impurities is separated with filtrate, obtain purified inulin extracting solution by filtration under diminished pressure, plate-and-frame filter press or whizzer;
Select the inorganic ultra-filtration membrane of tubular fibre of aperture 0.2um, remove thalline fully, solidify and water-soluble protein, colloid, pigment and other insolubles, and macroporous adsorbent resin decolouring, be that 0.001～0.01 electrodialysis ion-exchange membrane removes inorganic, the organic ion in the inulin solution with the aperture again, obtain refining inulin solution; Endo-inulinase hydrolysis (EC2.3.1.7), PH is 5.5, the time is 20h, obtains colourless no ash content content and be 1.013 kilograms of 86% oligofructoses.
Embodiment 3: produce high fructose syrup
Referring to Fig. 4, preparation method by above-mentioned high fructose syrup carries out, the squeezing of witloof heel piece, centrifugation with having soaked must contain 20% inulin liquid, adopt the secondary ions exchange, the first step is handed over resin with the Dowex88 highly acidic cation, the second stage is carried out removal of impurities with Dowex66 faintly acid anionite-exchange resin under 70 ℃ of temperature, in the product 12% of soluble substance, wherein 2.9% disaccharides, 71.4% fructose, 25.7% glucose.The product that obtains is evaporated to and contains 71% solid, obtains not having the ash free high fructose syrup of color.
Embodiment 4: production superelevation fructose syrup
Referring to Fig. 5, preparation method by above-mentioned superelevation fructose syrup carries out, with the hydrolysis under the effect of alantin excision enzyme (EC3.2.1.80) of inulin refined soln, temperature is 50 ℃, and the time is 2 hours, PH is 5-6, inulinase 0.15v/v, containing fructose in the hydrolysis of inulin liquid that obtains is 72%, is to be concentrated to original 20% under 65 ℃ with this hydrolyzed solution in temperature, the high fructose syrup solution of Huo Deing then, the concentration that is fructose is 92% superelevation fructose slurries.
Claims (3)
1. a witloof is hydrolyzed and produces the technology of fructose, it is characterized in that, adopts the inulin in the witloof to produce witloof plasmosin or superelevation fructose syrup or oligose or high fructose syrup, comprises the following steps:
The inulin of producing witloof plasmosin or superelevation fructose syrup or oligose extracts:
Root of Herba Cichorii crushing and water-adding after the Rapid Cleaning is soaked, 10 ℃-45 ℃ of water temperatures, the time is 20-30min; Or with the immersion of drying sheet root crushing and water-adding, 30 ℃-95 ℃ of water temperatures; Time is 20-60min, is heated to 75 ℃ of-100 ℃ of lixiviates then, and the time is 40min, carries out three adverse current lixiviates, after the washery slag operation, obtains thick aqueous extract; The inulin that is used to prepare plasmosin keeps former slag;
The inulin of producing high fructose syrup extracts:
Root of Herba Cichorii crushing and water-adding after the Rapid Cleaning is soaked, 10 ℃-45 ℃ of water temperatures, the time is 20-30min; Or with the immersion of drying sheet root crushing and water-adding, 30 ℃-95 ℃ of water temperatures; Time is 20-60min, and right using between its PH to 3.0-6.5 of acid accent under 30-75 ℃ of condition, placed 2 hours, filtered and regulate PH to 3.0-4.5 then, obtained hydrolysis material;
The preparation of described witloof plasmosin is undertaken by following step:
(1) fermentation: the thick aqueous extract that will obtain, inulinase direct hydrolysis in enzyme reactor, utilize endo-inulinase to regulate fermented liquid, can obtain the oligofructose solution of complete hydrolysis or partial hydrolysis at PH3.0-6.6, temperature 40-70 ℃, pol 25%, time 2-20 hour;
(2) enzyme that goes out: above-mentioned dreggy oligofructose solution is delivered to sterilization in the disinfection tank, and germ-resistant purpose is killed the arbitrary bacterium in the feed liquid and is made enzyme denaturation, 80 ℃～110 ℃ of Heating temperatures, time 5-15min, or select the higher temperature instantaneous sterilization, make protein coagulating, later cooling immediately;
(3) abrasive dust: the raw material behind the enzyme that will go out grinds processing, obtains pasty state solution;
(4) spraying drying: obtain pasty state solution and obtain powdery product, be the witloof plasmosin by spraying drying, forced air drying, drying bu sublimation.
The preparation of described superelevation fructose syrup or oligose is undertaken by following step:
(1) milk of lime is handled: the thick aqueous extract that is rich in inulin is cooled to 40-50 ℃, add milk of lime reagent at thick aqueous extract, and pH value transferred to 13.5, feed carbon dioxide then, protein, pectin and non-sugar colloid in the inulin crude extract are precipitated rapidly, and by filtration under diminished pressure, plate-and-frame filter press or whizzer precipitated impurities is separated with filtrate, obtain purified inulin extracting solution;
(2) enzyme that goes out is handled: the extracting solution that will be rich in inulin send and causes in the disinfection tank sterilization and make enzyme denaturation, solidifying protein, and Heating temperature is more than 90 ℃, below 110 ℃, time 5-15min, or select the higher temperature instantaneous sterilization, make protein coagulating, later cooling immediately;
(3) membrane filtration is removed thalline, water-soluble protein, pigment and other insolubles: select the aperture in 0.05-0.2 μ m or aperture the inorganic ultra-filtration membrane of tubular fibre at 0.05-0.1 μ m, remove thalline fully, solidify and water-soluble protein, colloid, pigment and other insolubles, obtain the clarifying aqueous extract that is rich in inulin;
(4) macroporous adsorbent resin decolouring: will pass through macroporous adsorbent resin through the aqueous extract that is rich in inulin of above-mentioned processing, and collect water elution liquid, and obtain inulin solution through decolouring;
(5) the electrodialysis ion-exchange membrane is handled: with the aperture is that 0.001～0.01 electrodialysis ion-exchange membrane removes inorganic, the organic ion in the inulin solution, obtains making with extra care inulin solution;
(6) to above-mentioned obtain refining inulin solution adopt endo-inulinase hydrolysis or alantin excision enzyme hydrolysis can obtain highly purified oligofructose or contain that fructose is 92%, glucose is less than 3% superelevation fructose syrup.
The preparation of described high fructose syrup is undertaken by following step:
(1) acid hydrolysis: the hydrolysis material that obtains is placed in the hydrolysis reactor, pH value between 3-6,120 ℃～160 ℃ of temperature, time 1-10min obtains hydrolysate;
(2) decolouring of high fructose syrup, desalination: hydrolysate at first ion-exchange gel chromatography removes by filter ash content, twice ion-exchange-resin process removes albumen then: earlier with strong acidic cation-exchange resin wash-out under greater than 70 ℃ condition, and then through weakly acidic cation-exchange resin, exchange by secondary ions, protein reduces 50% in the solution, dipolymer drops to 2.9% by 4.4%, and carbohydrate accounts for soluble material 12%; At last by gac formula charcoal bed depigmentation;
(3) collect solid: under the decompression situation, 50-100 ℃ concentrates, or 100-120 ℃ of normal pressure is concentrated, and the time is no more than 1 hour, and drying bu sublimation can obtain high fructose syrup then.
2. technology as claimed in claim 1 is characterized in that, the condition of described endo-inulinase hydrolysis is: 42 ℃-80 ℃ of fermented liquid temperature, and the PH of solution is 5-6.5, inulenin concentration 10%-30%, enzyme effect dosage are (2-30) U/g, time 6-30 hour; After the endo-inulinase hydrolysis, 90-120 ℃ went out enzyme 1-5 minute.
3. technology as claimed in claim 1, it is characterized in that, the condition of described alantin excision enzyme hydrolysis is: 50 ℃-65 ℃ of temperature, and PH is 5-6, the time is 1-5 hour, and the alantin excision enzyme of adding 0.15v/v, containing fructose in the liquid syrup that obtains is 72%, and glucose is 28%, colourless slurries, then above-mentioned slurries are concentrated to original 20%, the transparent golden yellow slurries that promptly obtain.
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| CN105886671A (en) * | 2016-02-26 | 2016-08-24 | 广西大学 | Clearing device for producing crystalline fructose with raw sugar as raw material |
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| CN109234336A (en) * | 2018-11-30 | 2019-01-18 | 中诺生物科技发展江苏有限公司 | A kind of method of dextrase enzymolysis inulin production oligofructose |
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