CN106318848B - A kind of device for being used to remove the D-Fructose in D-Psicose - Google Patents
A kind of device for being used to remove the D-Fructose in D-Psicose Download PDFInfo
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- CN106318848B CN106318848B CN201610900045.3A CN201610900045A CN106318848B CN 106318848 B CN106318848 B CN 106318848B CN 201610900045 A CN201610900045 A CN 201610900045A CN 106318848 B CN106318848 B CN 106318848B
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- C12M47/00—Means for after-treatment of the produced biomass or of the fermentation or metabolic products, e.g. storage of biomass
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Abstract
The invention discloses the device for removing the D fructose in D psicoses, it is made of isomerization system, oxidative system, piece-rate system, storage tank and collecting tank, wherein the bioreactor of glucose isomerase is dosed in the inside that the isomerization system is temperature control type；The oxidative system is that the bioreactor of glucose oxidase is dosed in the inside of temperature control type；The piece-rate system is to dose the chromatographic separator of alkalescence anion-exchange resin, and each system and tank, which are linked in sequence, constitutes complete circulating system.Apparatus of the present invention assemble simple and fast, it is easy to use, solve the problems, such as by D fructose extremely close with its property in D psicoses separate except, avoid the adjusting of pH and the rise of ion concentration in operating process at the same time, be conducive to being further purified for product, the additional utilization of byproduct gluconic acid is realized, is had a extensive future.
Description
Technical field
The present invention provides a kind of device of the D-Fructose efficiently removed in D-Psicose, belong to light equipment manufacture skill
Art field.
Background technology
Rare sugar is a kind of important carbohydrate, is played in meals, health care, medicine and other fields very important
Function.D-Psicose is that nature has few rare sugar, is nearly free from heat after edible, is low calorie sweetener.
It also has reduction blood glucose, reduces the important physiological functions such as blood fat, scavenging capacity oxygen radical and neuroprotection, its unique work(
Can and medical value cause extensive concern, be one of functional sugar research hotspot in recent years.Since D-Psicose is in nature
Content it is few, extraction is extremely difficult, and the method accessory substance of chemical synthesis is more, not easy purification, there is many drawbacks；And biosynthesis
Method still rest on laboratory level；And due to the substrate fructose or glucose and A Luo of production later stage production psicose
The property of ketose and its close so that isolating and purifying for later stage psicose is extremely difficult；These reasons cause psicose
The market price is expensive, mainly meets scientific research demand at present, is sold as reagent.
Although the market demand of psicose increasingly increases, fancy price limits their market scale and should
With.Therefore, production cost is greatly reduced, accomplishing scale production becomes of crucial importance.Using enzyme engineering technology, using fructose as original
Material can reduce the production cost of psicose using biological catalysis synthesis psicose, but react approximately half of during balance
Fructose is not converted, it is necessary to high-purity psicose could be arrived by being removed, but the property extremely phase of fructose and psicose
Closely, it is difficult to which the two is separated, usually used chromatographic separation technology, cost are higher at present.Therefore, research and development letter
Single, low cost psicose isolates and purifies device for simplifying production technology, reduces production cost, realizes heavy industrialization
Production is of great significance.
The content of the invention
In view of the problems of the existing technology, it is used to remove in D-Psicose the object of the present invention is to provide a kind of
The device of D-Fructose, be converted into D-Fructose while efficiently separating purifying D-Psicose to realize easily has economy by separated
The product of value.
The device of the present invention for being used to remove the D-Fructose in D-Psicose is by isomerization system 1, oxidative system
2nd, piece-rate system 3, storage tank 4 and collecting tank 5 form, wherein by liquid between the isomerization system, oxidative system, piece-rate system
Conveyance conduit is sequentially connected, and forms circulating system；
It is characterized in that：
The isomerization system is the container with jacket layer, and the container of jacket layer parcel is to have dosed solid glucose isomery
The reaction vessel 6 of enzyme, the container are provided with injection port 8 and outlet 9, its outlet is by being connected with the delivery pipe of liquid delivery pump 19
Road is connected to the injection port 12 of oxidative system, is full of recirculated water in the interlayer of jacket layer, circulating water temperature is adjusted by temperature regulating device 7
Control；The oxidative system is the container with jacket layer, and the container of jacket layer parcel is dose solid glucose oxidizing ferment anti-
Container 10 is answered, which is provided with injection port 12 and outlet 13, its outlet is by being connected with the delivery pipe of liquid delivery pump 20
Road is connected to the injection port 15 of piece-rate system, is full of recirculated water in the interlayer of jacket layer, circulating water temperature is adjusted by temperature regulating device 11
Control；The piece-rate system is to dose the separation vessel 14 of alkalescence anion-exchange resin, which is provided with injection port
15 and the outlet 16 with three-port structure, one of outlet isomery is connected to by the conveyance conduit for being connected with liquid delivery pump 18
The injection port 8 of change system, another exports the tank mouth that collecting tank 5 is connected to by the conveyance conduit for being connected with liquid delivery pump 21；Institute
State storage tank and be provided with the liquid delivery pump 17 that conversion fluid can be transported to isomerization system injection port 8；Above-mentioned each system and tank are suitable
Sequence has connected and composed complete circulating system.
In the above-mentioned device for removing the D-Fructose in D-Psicose：The isomerization system is preferably by glass system
Into being in the form of a column, circulation in its overcoat layer interlayer connection water-bath, the temperature regulating device utilizes water-bath regulation and control circulation
Coolant-temperature gage realizes that institute's controlling temperature is 65 DEG C.
In the above-mentioned device for removing the D-Fructose in D-Psicose：The oxidative system is preferably made of glass,
It is in the form of a column, the circulation connection water-bath in its overcoat layer interlayer, the temperature regulating device utilizes water-bath regulation and control recirculated water
Temperature realizes that institute's controlling temperature is 40 DEG C.
In the above-mentioned device for removing the D-Fructose in D-Psicose：The alkalescence anion-exchange resin is preferably
Macropore polystyrene weak-base anion-exchange resin.
In the above-mentioned device for removing the D-Fructose in D-Psicose：The storage tank is to be used to store D-Fructose and D-
The tank body of psicose mixed solution, is preferably made of stainless steel, glass or ceramics.
In the above-mentioned device for removing the D-Fructose in D-Psicose：The collecting tank is to be used to collect high concentration D-
The tank body of psicose solution, is preferably made of stainless steel, glass or ceramics.
The device of the present invention for being used to remove the D-Fructose in D-Psicose is in separation D-Fructose and D-Psicose
In application.
The invention discloses a kind of device for being used to remove the D-Fructose in D-Psicose, experiment confirms：Utilize the dress
Put by the continuous circular treatment of conversion fluid, can effectively be separated fructose converting for gluconic acid, solving property
Two kinds of extremely close sugar of matter are difficult to the problem of separation, and since the gluconic acid of generation constantly being separated, no
Need plus alkali controls pH, reaction solution ions content is low, is easy to subsequent purification；Whole simple production process, production cost are notable
Reduce, to realize large-scale industrial production, realize that volume production, high yield are laid a good foundation.
To sum up, the invention has the advantages that：
(1) using apparatus of the present invention by the continuous circular treatment of conversion fluid, effectively can finally convert fructose
It is separated off for gluconic acid and with resin adsorption, solves the extremely close fructose of property and psicose is difficult to separated ask
Topic；
(2) continuous circular treatment, solves glucose isomerase enzyme and promotees the drawbacks of reaction is reversible so that react to generation
The direction of glucose carries out, and make use of glucose isomerase to greatest extent；
(3) ion exchange resin absorption gluconic acid further solves the problems, such as reacting liquid pH value adjusting, avoids
The rise of ion concentration, and whole process can be with serialization；
(4) gluconic acid adsorbed in ion exchange resin column can utilize hydrochloric acid (sodium chloride/calcium chloride/zinc chloride) to solve
Inhale, obtain gluconic acid (sodium gluconate/calcium/zinc), can increase profit, the receipts of increase psicose production as coproduction product
Benefit.
Brief description of the drawings
Fig. 1 is the structure diagram of the present invention for being used to remove the D-Fructose device in D-Psicose；
Wherein：1 is isomerization system, and 2 be oxidative system, and 3 be piece-rate system, and 4 be storage tank, and 5 be collecting tank, and 6 be isomery
Change system response device, 7 be isomerization system temperature regulating device, and 8 be isomerization system reactor injection port, and 9 is anti-for isomerization system
Device outlet is answered, 10 be oxidative system reactor, and 11 be oxidative system temperature regulating device, and 12 be oxidative system reactor injection port,
13 be oxidative system reactor outlet, and 14 be piece-rate system separator, and 15 be piece-rate system injection port, and 16 go out for piece-rate system
Sample mouth, 17~21 be liquid delivery pump.
Fig. 2 is high-efficient liquid phase analysis by the sample composition figure before and after circular treatment；
Wherein：22 be fructose content balance figure before and after the processing, and 23 be psicose content balance figure before and after the processing, 24 be Ah
Lip river ketose standard specimen.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1 is used for D-Fructose and D-Psicose separator
As shown in Figure 1.
For remove the device of the D-Fructose in D-Psicose by isomerization system 1, oxidative system 2, piece-rate system 3,
Storage tank 4 and collecting tank 5 form, wherein between the isomerization system, oxidative system, piece-rate system by liquid conducting pipes successively
Connection, forms circulating system；
Wherein：
The isomerization system is made of glass, the container with jacket layer being in the form of a column, and the container of jacket layer parcel is
The reaction vessel 6 of solid glucose isomerase is dosed, which is provided with injection port 8 and outlet 9, its outlet is by being connected with
The conveyance conduit of liquid delivery pump 19 is connected to the injection port 12 of oxidative system, is full of recirculated water in the interlayer of jacket layer, circulates
Water system connects water-bath, and temperature regulating device 7 realizes that institute's controlling temperature is 65 DEG C using water-bath regulation and control circulating water temperature；The oxygen
Change system is made of glass, the container with jacket layer being in the form of a column, and the container of jacket layer parcel is to have dosed solid glucose
The reaction vessel 10 of oxidizing ferment, the container are provided with injection port 12 and outlet 13, its outlet is by being connected with liquid delivery pump
20 conveyance conduit is connected to the injection port 15 of piece-rate system, and recirculated water, circulation connection are full of in the interlayer of jacket layer
Water-bath, temperature regulating device 11 realize that institute's controlling temperature is 40 DEG C using water-bath regulation and control circulating water temperature；The piece-rate system is
The separation vessel 14 of macropore polystyrene weak-base anion-exchange resin is dosed, which is provided with injection port 15 and tool
There is the outlet 16 of three-port structure, one of outlet is connected to isomerization system by the conveyance conduit for being connected with liquid delivery pump 18
Injection port 8, another, which is exported, is connected to the tank mouth of collecting tank 5 by the conveyance conduit for being connected with liquid delivery pump 21；The collection
Tank is the tank body for collecting high concentration D-Psicose solution, is made of stainless steel, glass or ceramics；The preserving jar is to use
In storage D-Fructose and the tank body of D-Psicose mixed solution, it is made of stainless steel, glass or ceramics, it, which is provided with, will turn
Change the liquid delivery pump 17 that liquid is transported to isomerization system injection port 8；Above-mentioned each system and tank, which are linked in sequence, to be constituted completely
Circulating system.
Embodiment 2 realizes the removal of the D-Fructose in D-Psicose using 1 described device of embodiment
(1) pretreatment of alkalescence anion-exchange resin：Processing method is with reference to country of the GB5476-85 People's Republic of China (PRC)
Standard ion exchange resins preprocess method；
1. resin is fitted into the chromatographic column that internal diameter is 3cm, column bed height is 30cm, is rinsed repeatedly with pure water, directly
Into sample without visible mechanical admixture and untill going out clarification of water；
2. 100mL 1N hydrochloric acid solutions, 200mL pure water, 100mL1N sodium hydroxide solutions and 200mL pure water are used successively, from
Above lower to pass through resin bed, reagent flow 2.0mL/min, pure water flow is 10mL/min, in each transferring reagent, makes liquid
Face is higher by resin bed 1cm, ensures bubble-free in resin bed；This operation carries out 2 times；
3. through 2. processed resin with 400mL 1N sodium hydroxide solutions by resin bed, flow 10mL/min, so
Pure water is used afterwards, until stopping washing when being colourless with instructions phenolphthalein solution inspection efflux；
(2) fructose soln of final concentration of 550g/L is prepared with distilled water；
(3) using solid D-Psicose 3- epimerases as catalyst, urged by 55g is added in every 100mL fructose solns
The ratio of agent adds the catalyst into fructose soln, and catalyst is separated off after reacting 5h at 68 DEG C, obtain containing D- Ah
The conversion fluid of Lip river ketose and D-Fructose, conversion fluid are positioned over the storage tank of separator；
(4) conversion fluid containing fructose and psicose, the sample introduction that isomerization system is passed through with the flow velocity of 5mL/min in storage tank
Mouth flow to the internal-response container in isomerization system, is realized by the processing of isomerization system reactor by part in conversion fluid
D-Fructose is converted into D-Glucose, obtains the mixed solution containing D-Fructose, D-Glucose and D-Psicose；
(5) mixed solution is flowed out by the outlet of isomerization system, then passes through oxidative system sample introduction with the flow velocity of 5mL/min
Mouth flows into oxidative system internal-response container；Processing through two reaction vessels, is realized D-Glucose whole in mixed liquor
Gluconic acid is converted into, the mixed solution containing fructose and psicose becomes the mixing containing fructose, gluconic acid and psicose
Solution；
(6) mixed solution containing fructose, gluconic acid and psicose is flowed out by the outlet of oxidative system, with 3mL/
The flow velocity of min flows into separation vessel inside piece-rate system by the injection port of piece-rate system, by alkalescence anion-exchange resin
Suction-operated by gluconic acid adsorb remove；
(7) mixed solution is flowed out by piece-rate system outlet, again with the flow velocity of 5mL/min by isomerization system into
Sample mouth flow to the internal-response container in isomerization system；
(8) according to the method repetitive operation of step (4) (5) (6) (7), circulate 13 times, by piece-rate system another with receipts
Collect the solution of outlet outflow D-Psicose containing high concentration of tank tank mouth docking.
Sample composition of the high-efficient liquid phase analysis after circular treatment, the purity of psicose can reach 95%, the result is shown in
Fig. 2.
The crystallization of 3 D-Psicose of embodiment
Handle the obtained solution of the D-Psicose containing high concentration by embodiment 2, using falling temperature method crystallize to obtain D- Ah
Lip river ketose crystalline solid.Embodiment is as follows：
The liquid glucose that embodiment 2 obtains is dried to obtain to the psicose sugar juice of saturation using vacuum drying method, will
After liquid glucose is heated to 65 DEG C, with volume ratio 1：4 ratio adds acetone soln, psicose crystal seed is then added, with 4 DEG C/min
Speed cooling, be down to 4 DEG C, obtain the crystalline solid of psicose.
The desorption of 4 gluconic acid of embodiment
(1) dilute hydrochloric acid of final concentration of 0.5mol/L is prepared；
(2) after embodiment 1, with the flow velocity of 2mL/min by the dilute hydrochloric acid of 100mL 0.5mol/L by piece-rate system
Injection port flows into；
(3) gluconic acid solution that the liquid flowed out by piece-rate system outlet obtains for desorption, gluconic acid is as connection
Production product can increase profit, the income of increase psicose production.
By circular treatment, the removal rate of the D-Fructose in conversion fluid can reach more than 95%.To sum up, the method for the present invention
It is simple and easy to use, the production cost of D-Psicose can be greatly reduced, there is huge industrial applications prospect.
Claims (7)
1. a kind of device for being used to remove the D-Fructose in D-Psicose, described device includes isomerization system (1), oxidation system
System (2), piece-rate system (3), storage tank (4) and collecting tank (5), wherein between the isomerization system, oxidative system, piece-rate system
It is sequentially connected by liquid conducting pipes, forms circulating system；
It is characterized in that：
The isomerization system is the container with jacket layer, and the container of jacket layer parcel is to dose solid glucose isomerase
Reaction vessel (6), the container are provided with injection port (8) and outlet (9), its outlet is by being connected with the defeated of liquid delivery pump (19)
The injection port (12) that pipeline is connected to oxidative system is sent, is full of recirculated water in the interlayer of jacket layer, circulating water temperature is filled by temperature control
Put (7) regulation and control；The oxidative system is the container with jacket layer, and the container of jacket layer parcel is to have dosed solid glucose oxidation
The reaction vessel (10) of enzyme, the container are provided with injection port (12) and outlet (13), its outlet is conveyed by being connected with liquid
The conveyance conduit of pump (20) is connected to the injection port (15) of piece-rate system, is full of recirculated water, circulating water temperature in the interlayer of jacket layer
Degree is regulated and controled by temperature regulating device (11)；The piece-rate system is to dose the separation vessel of alkalescence anion-exchange resin (14),
The separation vessel is provided with injection port (15) and the outlet (16) with three-port structure, and one of outlet is defeated by being connected with liquid
The conveyance conduit of pump (18) is sent to be connected to the injection port (8) of isomerization system, another outlet is by being connected with liquid delivery pump (21)
Conveyance conduit be connected to the tank mouths of collecting tank (5)；The storage tank, which is provided with, can be transported to conversion fluid isomerization system sample introduction
The liquid delivery pump (17) of mouth (8)；Above-mentioned each system and tank, which are linked in sequence, constitutes complete circulating system.
2. the device as claimed in claim 1 for being used to remove the D-Fructose in D-Psicose, it is characterised in that：The isomery
Change system is made of glass, is in the form of a column, and the circulation connection water-bath in its overcoat layer interlayer, the temperature regulating device utilizes
Water-bath regulation and control circulating water temperature realizes temperature control, and institute's controlling temperature is 65 DEG C.
3. the device as claimed in claim 1 for being used to remove the D-Fructose in D-Psicose, it is characterised in that：The oxidation
System is made of glass, is in the form of a column, and the circulation connection water-bath in its overcoat layer interlayer, the temperature regulating device utilizes water
Bath regulation and control circulating water temperature realizes temperature control, and institute's controlling temperature is 40 DEG C.
4. the device as claimed in claim 1 for being used to remove the D-Fructose in D-Psicose, it is characterised in that：The alkalescence
Anion exchange resin is macropore polystyrene weak-base anion-exchange resin.
5. the device as claimed in claim 1 for being used to remove the D-Fructose in D-Psicose, it is characterised in that：The storage tank
It is the tank body for storing D-Fructose and D-Psicose mixed solution, is made of stainless steel, glass or ceramics.
6. the device as claimed in claim 1 for being used to remove the D-Fructose in D-Psicose, it is characterised in that：The collection
Tank is the tank body for collecting high concentration D-Psicose solution, is made of stainless steel, glass or ceramics.
7. the device for being used to remove the D-Fructose in D-Psicose described in claim 1 is in separation D-Fructose and D- A Luo ketone
Application in sugar.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106480125A (en) * | 2016-10-14 | 2017-03-08 | 山东大学 | A kind of method that low cost produces D psicose |
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| JP4627841B2 (en) * | 2000-06-08 | 2011-02-09 | 国立大学法人 香川大学 | Psicose separation method |
| DK2401046T3 (en) * | 2009-02-25 | 2020-08-03 | Dupont Nutrition Biosci Aps | SEPARATION PROCESS |
| CN102020680B (en) * | 2011-01-07 | 2012-05-02 | 保龄宝生物股份有限公司 | Method for preparing high-purity lactulose |
| KR20160062349A (en) * | 2014-11-25 | 2016-06-02 | 씨제이제일제당 (주) | A method of manufacturing high purity d-psicose |
| CN105256079A (en) * | 2015-10-22 | 2016-01-20 | 林树仁 | Purification method for HFCS (high fructose corn syrup) in fructose production process |
| CN105734092B (en) * | 2016-05-06 | 2019-07-16 | 江苏中酶生物科技有限公司 | A kind of method that enzyme process prepares D-Tag |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106480125A (en) * | 2016-10-14 | 2017-03-08 | 山东大学 | A kind of method that low cost produces D psicose |
| CN106480125B (en) * | 2016-10-14 | 2019-05-21 | 山东大学 | A method of producing D-Psicose |
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