CN109734756A - A kind of method of chromatographic isolation maltitol - Google Patents
A kind of method of chromatographic isolation maltitol Download PDFInfo
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- CN109734756A CN109734756A CN201910150851.7A CN201910150851A CN109734756A CN 109734756 A CN109734756 A CN 109734756A CN 201910150851 A CN201910150851 A CN 201910150851A CN 109734756 A CN109734756 A CN 109734756A
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- maltitol
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- chromatographic isolation
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Abstract
The invention belongs to the technical field of maltitol separation, specially a kind of methods of chromatographic isolation maltitol.Liquid material to be separated will be needed to separate by chromatographic fractionation system, so that the concentration of maltitol component is mentioned to 95% after separation, then directly concentration carries out primary crystallization, obtains crystal maltitol product, and guarantee total recovery.Method of the invention is in optimized selection the parameter in separation process by using chromatographic fractionation system, obtains a kind of convenient for operation, at low cost, the method for the high acquisition maltitol of product quality.
Description
Technical field
The invention belongs to the technical field of maltitol separation, specially a kind of methods of chromatographic isolation maltitol.
Background technique
Maltitol is a kind of novel functional sweetener, due to its with low in calories, non-saprodontia, indigestible,
Promote a variety of physiological properties such as the absorption of calcium, causes the extensive concern of people.Maltitol also known as hydrogenated maltose,
Chemical name is 4-O- alpha-D-glucose base-D- glucitol, molecular formula C12H24O11, relative molecular mass 344.31.Malt
Sugar alcohol be white crystalline powder or colorless and transparent neutral thick liquid, it is soluble easily in water, do not dissolve in methanol and ethyl alcohol.Hygroscopicity
Very strong, maltitol sugariness is the 90% of sucrose, excellent flavor.Maltitol calorific value only has 2.1 cards/g, can inhibit body fat
Surplus accumulation.Maltitol does not contain aldehyde radical, and no reduction has better heat resistance than sucrose.Maltitol is than all
Saccharic all hardly possiblies are greatly improved the storage life of food by microbial assimilation and utilization.Maltitol does not participate in metabolism directly, will not
Directly increase blood glucose, do not increase cholesterol, is the ideal sweetener of remedy diet.It, can anti-caries for infant foods.
Crystal maltitol can be applied in pharmaceuticals industry, since the hydrolysis rate of maltitol in vivo is very slow, people
Body takes in the blood glucose level and blood insulin level increasing degree very little after maltitol, can be used for as this spy of diabetes patient
The raw materials of food processing of different crowd;The medicine such as production injection syrup can be processed after specially treated using crystal maltitol
Product;Maltitol can also promote the absorption of calcium, can be processed into drink, and it is hard to be exclusively used in diabetes, hepatopathy, cardiovascular disease, artery
Change, hypertension, obesity and patients with osteoporosis food demand.
It is industrial that maltitol can be applied in sugarfree foods, and in moon cake manufacturing process, maltitol is added it
In can be made into sugar-free moon cake, as a kind of health-care moon cake, sugar-free moon cake sugariness is slightly lower, do not cause blood glucose rise after edible, and
Mouthfeel is also different from traditional mooncake.Crystal maltitol makes as sweetener in the solid-state foods such as sugar-free biscuit, old people food
With not only heat is low, and in good taste, sales volume is also improving year by year.
The development of China's maltitol is started late, and starts the 1970s to develop, and by the development of many years, is produced at present
Amount, kind, quality all obtain very big development, as the improvement of people's living standards, people increasingly pay close attention to diet to itself
The influence of the general level of the health, the propensity to consume are increasingly turned to the functional food with adequate nutrition and health, and sales volume improves year by year,
About 60,000 tons/year or more of production capacity has been formed at present.To the end of the year 2013, maltitol market demand total amount was compared with 2009
It increases more than 2.5 times, and crystal maltitol is with its shelf-stable, convenient transportation, product content is high, is conducive to solid-state food use
The advantages that usage amount can be more and more, crystalline product is mainly used for exporting at present, with domestic consumption amount increase and production skill
The raising of art, production cost can gradually reduce, and the use amplitude of crystal maltitol can increase year by year.
The production technology of maltitol:
Maltitol is the disaccharide alcohol made of maltose hydrogenated reduction.Its industrial production technology can be divided into two big portions
Point, first part is that Starch Hydrolysis is made to high maltose syrup, and second part is made of by malt syrup hydrogenating reduction obtained
Maltitol.Entire process flow: starch-size mixing (concentration 10%~20%, pH6.0~6.4)-liquefaction (100 DEG C, DE10~
12)-saccharification (45~50 DEG C, pH5.8~6.0)-filters pressing-decoloration (pH4.5~5.0,80 DEG C, 30rain, 20~25 revs/min)-
Filters pressing-ion exchange (flow velocity 700kg/h, 40cI=or so)-is concentrated in vacuo (0.086~0.092Mpa, 50~53 DEG C)-Gao Mai
Bud syrup-stock (concentration 12%~15%)-tune pH (7.5~8.0)-charging reaction (120 DEG C~130 DEG C of temperature, pressure
8Mpa)-filtering decoloration-ion exchange-evaporation and concentration-finished product.
Before not using chromatographic isolation, generally all guarantee the quality and receipts of crystalline maltose by second-crystallized method
Rate.Crystallization for the first time guarantees the bottom sugar purity formally crystallized for the second time, and second of crystallization guarantees to produce qualified crystal malt
Sugar product.Specific method: by forced circulation continuous crystallization method or using pre-crystallized+crystallisation by cooling method to 80% maltitol into
Row primary crystallization, wet sugar can be not required to wash, and first then the massecuite of acquisition 95% carries out heating dissolution to bottom sugar and go two as bottom sugar
Secondary crystallization, using separation, the qualified crystalline product of dry acquisition, and the mother liquor after separating can go production liquid maltitol to produce
Product.
Second-crystallized method process is as follows:
Although second-crystallized method can produce qualified crystal maltitol, process is long, and qualifying point is more, not only produces
At high cost, product quality is also difficult to control.
Crystallisation produce crystal maltitol, have one on condition that how to obtain high-purity bottom sugar because in substrate
Influence of the maltitol content to crystallization yield is bigger.We can pass through data comparison explanation in the following table 1.
1 substrate purity of table and yield relation table
Product purity, % | Bottom sugar purity, % | Mother liquor purity, % | Yield, % |
99.5 | 95.0 | 75.0 | 85.50 |
99.5 | 93.0 | 75.0 | 78.60 |
99.5 | 91.0 | 75.0 | 71.41 |
99.5 | 89.0 | 75.0 | 63.88 |
99.5 | 87.0 | 75.0 | 56.02 |
99.5 | 85.0 | 75.0 | 47.78 |
99.5 | 83.0 | 75.0 | 39.14 |
99.5 | 81.0 | 75.0 | 30.08 |
99.5 | 79.0 | 75.0 | 20.56 |
From table 1 it will be seen that in the case where product purity is as mother liquor content, substrate kind compositional purity pair
Yield bring influences very big, if decrystallized product with the bottom sugar of low-purity, can also generate following situations: product component contains
Measure that low, product particle degree is small, mother liquor separates that difficult dry yield is low, operating cost is high.
It is had the following disadvantages by second-crystallized method production, the period is long, process is more, labour cost is high, production cost height etc.
Objective circumstances.Because process is more, control point increases, it is easy to affect product quality.
Summary of the invention
It is an object of the invention to the high requests and product particle degree for above-mentioned second-crystallized method for bottom sugar purity
The problems such as small problem, complex process, high operating cost, provide a kind of method of chromatographic isolation maltitol.
The technical solution of the present invention is as follows:
A kind of method of chromatographic isolation maltitol, will need liquid material to be separated to be divided by chromatographic fractionation system
From so that the concentration of maltitol component is mentioned to 95% after separation, then directly concentration carries out primary crystallization, obtains crystal malt
Sugar alcohol product.
The features of the present invention is also:
The raw material of the liquid maltitol forms: sorbierite 2.0~5%, maltitol 60~68%, maltotriose alcohol 15
~20%, polyalcohol 10-11.5%.
Further preferably, the raw material composition of the liquid maltitol: sorbierite 2.0~3%, maltitol 60~68%,
Maltotriose alcohol 15~20%, polyalcohol 10-11.5%, sorbierite belong to most slow component in chromatographic concentrations bands of a spectrum, and malt
Sugar alcohol also belongs to slow component, to obtain the maltitol product of high-purity, and the sorbitol content that should be controlled in raw material is unsuitable excessively high,
To be advisable lower than 3%.
Into the input concentration 58-60% of the need liquid material to be separated in chromatographic fractionation system, conductivity≤20cm/
S, 65 DEG C of feeding temperature, the column temperature in control system is 60-65 DEG C, and the pressure in system is 0.5-0.55Mpa.By control into
Expect concentration, conductivity, column temperature, pressure and other parameters, further improves the content concn of maltitol obtained after separation, be convenient for
Impurity is washed off, to obtain high-purity extracting solution.
In chromatographic fractionation system, using circulation back pressure feed system, it can be achieved that smooth continuous feed, is below discharging system
System, input and output material are all made of the switching that pneumatic on-off valve carries out input and output material by process control.
In the chromatographic fractionation system, the unit by resin filling continuously recycled by 4-6 is formed, preferably 4 companies
The unit by resin filling of continuous circulation forms, and in 4 units, liquid material to be separated is needed continuously to flow to from tower top
Then bottom again returns to the top of next unit.
Further, the resin is Ca2+Type ion exchange resin, feed flow rate 4.0-5.0mL/min, elution flow rate
7.5mL/min, switching time 300-400s, by selecting reasonable resin type, the parameter of control feed flow rate etc., realization pair
The separation preparation work of maltitol obtains purity is high, high-quality product.
Further, in the chromatographic fractionation system, using desalted water as elutriant, the conductivity of desalted water is less than 5cm/
s。
The invention has the benefit that
The method of chromatographic isolation maltitol of the invention, by chromatographic fractionation system by the purity of maltitol component from
80% once mentions to 95% or so, and product basically reaches the purity requirement of crystallization substrate, and process of decrystallizing can directly be concentrated, and
And guarantee total recovery.
In above-mentioned process, sorbierite belongs to most slow component in chromatographic concentrations bands of a spectrum, and maltitol also belongs to
In slow component, the maltitol product of high-purity is obtained, the unsuitable excessively high control of sorbitol content in raw material should be controlled in 2-
5%, to be advisable lower than 3%.
In short, method of the invention optimizes choosing to the parameter in separation process by using chromatographic fractionation system
It selects, obtains a kind of convenient for operation, at low cost, the method for the high acquisition maltitol of product quality.
Detailed description of the invention
Fig. 1 is the process flow chart of the method for chromatographic isolation maltitol of the present invention.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, below in conjunction with of the invention real
The attached drawing in example is applied, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work, all should belong to protection of the present invention
Range.
It can be seen that, D, F be to recycle back pressure feed system, it can be achieved that smooth continuous feed, below for out in conjunction with attached drawing 1
Material system, input and output material are all made of the switching that pneumatic on-off valve carries out input and output material by process control, and chromatography point is specifically described below
From principle and autocontrol operation mode.
A. sequential simulated moving bed principle
Sequential simulated moving bed is a continuous chromatographic isolation technique, it be continuously recycled by 4-6 have tree
The unit composition of rouge (stationary phase) filling.Since the separation equipment is to simulate resin by the periodical replacement of inlet and outlet
(movement) is replaced, so being referred to as " Simulation moving bed ".
In 4 units, needs liquid to be separated continuously to flow to bottom from tower top, then again return to next unit
Top.The direction of liquid migration is consistent in the chromatographic band of concentration of component and chromatographic column in expression system.When chromatographic band is complete
When length of the portion Jing Guo a chromatographic column, which is just completed.As chromatographic band moves in system, material import and export also with
Move on to next position.In this way, position and the chromatographic concentrations bands of a spectrum in system of inlet and outlet remain it is opposite consistent.It is connecing
Inlet and outlet position is fixed in the chromatographic band to get off the mobile time, and until next time, chromatographic band passes fully through this section of chromatographic column
When inlet and outlet switch over therewith again.The time switched every time is just called sequential time.
Continuous circular flow is referred to as circuit flow, and related with this circuit flow there are also four additional flow, tools
Body is as follows.
Feed rate: refer to the feed rate of high malt sugar alcohol slurry, this must be handled in chromatographic isolation unit.
Elution flow quantity: refer to that elution flow quantity required for separation (herein refers to the process water of degassing, this is that this is
Second of charging of system).
Extract flow quantity: refer to has the rate of discharge of the very product of strong affinity (to herein refer to malt with fixed mediums
The rate of discharge of sugar alcohol).
Raffinate flow: refer to the product most weak with fixed mediums affinity rate of discharge (herein refer to sorbierite and
The rate of discharge of DP3-n).
B. process operation
In SSMB (sequential type simulated moving bed chromatography separating technology) technique, each mutually stream is no longer continuous, but a week
Each step in phase is all divided into 4 substeps (A-B-C-D).
Here be in relation in technique in the first step 4 substeps (A-B-C-D) description.
SSMB technique can generally use circuit flow (or elution water flow), feed rate, and each substep has one
Period, totally 4 cycle Ts A, TB, TC and TD.Step C and step D are started simultaneously at.So in cycles, extraction is constantly isolated
Liquid (component rich in maltitol) and raffinate (component of low content maltitol, sorbierite/DP (3-n)).
Embodiment 1
In order to verify feasibility and economy of the method in separating maltitol of chromatographic isolation maltitol of the invention,
Cooperate to carry out small industrialization chromatographic isolation examination with hundred garden Long Chuan of Shandong.
A kind of method of chromatographic isolation maltitol of the invention will need liquid material to be separated to pass through chromatographic isolation system
System is separated, so that the concentration of maltitol component is mentioned to 95% after separation, then directly concentration carries out primary crystallization, obtains
Crystal maltitol product.
In chromatographic fractionation system, using circulation back pressure feed system, it can be achieved that smooth continuous feed, is below discharging system
System, input and output material are all made of the switching that pneumatic on-off valve carries out input and output material by process control.
The simple process uses automatic control system, is suitble to continuous production process.
In order to verify method of the invention in the feasibility for improving crystal maltitol substrate purity, we pass through small-sized work
Industry chromatographic system carries out separation test, obtains good refining effect.
1. the maltitol separation test condition carried out
(1) the small industrialization chromatographic system scale of: day handles 1 ton of maltitol butt raw material;
(2) raw material forms: sorbierite 2.0%, maltitol 68%, maltotriose alcohol 18.7%, polyalcohol 11.3%;
Unite water consumption: processing 1 ton of butt 60% maltitol raw material need 2.6 tons of desalted waters of water consumption, desalted water conductance
Within rate 5cm/s;
(4) input concentration 60%, conductivity 20cm/s, 65 DEG C of feeding temperature, column temperature is 63-65 DEG C, and pressure is
0.55Mpa;
(5) 4 units by resin filling continuously recycled form, resin Ca2+Type ion exchange resin, feeding flow
Fast 5.0mL/min, elution flow rate 7.5mL/min, switching time 350s.
Following table 2 is the mask data of every 3 hours of acquisition after system stable operation.
The small industrialization chromatographic isolation analysis record of 2 Shandong of table, hundred garden Long Chuan sugar alcohol
In terms of the average value of this group of separating resulting, average purity reaches 95%, and product purity basically reaches crystallization substrate
Purity requirement, and mask data is reliable and stable.
Test example 1
The sugar alcohol separation test situation that green strong biotechnology carries out in Yucheng
For the separating effect for verifying different product, the applicant carries out in Yucheng, Shandong Lv Jian Biotechnology Co., Ltd
Maltitol separation test.
Experimental condition is as follows:
Small industrialization chromatographic system scale: day handles 1 ton of maltitol butt raw material;
Raw material composition: sorbierite 6.5%, maltitol 67.8%, maltotriose alcohol 15.5%, polyalcohol 10.2%;
Input concentration: 58%;Conductivity: within 20cm/s;65 DEG C of feeding temperature, the column temperature in control system is 65 DEG C,
Pressure in system is 0.5Mpa;
System water consumption: the maltitol raw material of 1 ton of butt 60% of processing needs 2.8 tons of desalted waters of water consumption;Conductivity: less than
5cm/s;Feeding temperature: 675 DEG C.
4 units by resin filling continuously recycled form, 4 unit groups for having resin to fill continuously recycled
At resin Ca2+Type ion exchange resin, feed flow rate 5.0mL/min, elution flow rate 7.5mL/min, switching time 350s.
Table 3 is the small industrialization mask data of strong biotechnology raw material green to Yucheng
It is analyzed from above data, the purity 93.48% after average separation, yield 87.3%, which is lower than embodiment
1, tentatively meet maltitol crystallization processes requirement, but the separation purity of 100 garden Long Chuan of embodiment acquisition and yield are higher than the examination
The green strong separating effect of example 1 is tested, this is because the content of sorbierite and other alcohol is higher in green strong raw material.Because of sorbierite
Belong to most slow component in chromatographic concentrations bands of a spectrum, and maltitol also belongs to slow component, the maltitol that obtain high-purity produces
Product, the sorbitol content that should be controlled in raw material are unsuitable excessively high.
By the above embodiments and test example 1, it can be seen that, embodiment 1, product average purity reaches 95%, product base
Originally reach the purity requirement of crystallization substrate, and mask data is steady;Purity after the green arrow raw material separation of the separation of test example 1 is 9
3.48%, yield 87.3%, the average value tentatively meets maltitol crystallization processes requirement, this is because sorb in green strong raw material
The higher reason of the content of alcohol and other alcohol.Because sorbierite belongs to most slow component in chromatographic concentrations bands of a spectrum, and maltitol
Belong to slow component, to obtain the maltitol product of high-purity, the sorbitol content that should be controlled in raw material is unsuitable excessively high.
Claims (8)
1. a kind of method of chromatographic isolation maltitol, which is characterized in that liquid material to be separated will be needed to pass through chromatographic isolation
System is separated, so that the concentration of maltitol component is mentioned to 95% after separation, then directly concentration carries out primary crystallization, obtains
To crystal maltitol product.
2. the method for chromatographic isolation maltitol according to claim 1, which is characterized in that the original of the liquid maltitol
Material composition: sorbierite 2.0~5%, maltitol 60~68%, maltotriose alcohol 15~20%, polyalcohol 10-11.5%.
3. the method for chromatographic isolation maltitol according to claim 2, which is characterized in that the original of the liquid maltitol
Material composition: sorbierite 2.0~3%, maltitol 60~68%, maltotriose alcohol 15~20%, polyalcohol 10-11.5%.
4. the method for chromatographic isolation maltitol according to claim 1, which is characterized in that enter in chromatographic fractionation system
Need liquid material to be separated input concentration 58-60%, conductivity≤20cm/s, 65 DEG C of feeding temperature, in control system
Column temperature be 60-65 DEG C, the pressure in system is 0.5-0.55Mpa.
5. the method for chromatographic isolation maltitol according to claim 1, which is characterized in that in chromatographic fractionation system, adopt
It is below discharge system with circulation back pressure feed system, input and output material is all made of pneumatic on-off valve and is passed in and out by process control
The switching of material.
6. the method for chromatographic isolation maltitol according to claim 1, which is characterized in that in the chromatographic fractionation system,
The unit by resin filling continuously recycled by 4-6 forms, preferably 4 units for having resin to fill continuously recycled
Composition needs liquid material to be separated continuously to flow to bottom from tower top, then again returns to next list in 4 units
The top of member.
7. the method for chromatographic isolation maltitol according to claim 1, which is characterized in that the resin is Ca2+Type
Ion exchange resin, feed flow rate 4.0-5.0mL/min, elution flow rate 7.5mL/min, switching time 300-400s.
8. the method for chromatographic isolation maltitol according to claim 1, which is characterized in that in the chromatographic fractionation system,
Using desalted water as elutriant, the conductivity of desalted water is less than 5cm/s.
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Cited By (1)
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CN114249780A (en) * | 2021-12-23 | 2022-03-29 | 浙江华康药业股份有限公司 | Method for preparing liquid maltitol and liquid polyol by using maltitol chromatographic raffinate |
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