CN106366137A - Desalting and decolorizing method of isomerized lactose liquid - Google Patents
Desalting and decolorizing method of isomerized lactose liquid Download PDFInfo
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- CN106366137A CN106366137A CN201610739934.6A CN201610739934A CN106366137A CN 106366137 A CN106366137 A CN 106366137A CN 201610739934 A CN201610739934 A CN 201610739934A CN 106366137 A CN106366137 A CN 106366137A
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- lactose
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/04—Disaccharides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Abstract
The invention discloses a desalting and decolorizing method of isomerized lactose liquid. The desalting and decolorizing method comprises the following steps of (1) desalting and decolorizing the isomerized lactose liquid prepared by chemical isomerization of lactose by adopting a sequential simulated moving bed chromatography to obtain three components which are a salt component, an isomerized lactose component and a pigment component; and (2) carrying out decolorization and ion exchange resin desalination on the isomerized lactose component obtained in the first step to prepare a desalted and decolorized liquid isomerized lactose product. According to the desalting and decolorizing method, by adopting the sequential simulated moving bed chromatography to desalt the isomerized lactose liquid, the desalinization ratio reaches 85 percent or above, and the problems of rapid failure of ion exchange resin, frequent regeneration and low efficiency by only adopting an ion exchange method to carry out desalination are solved.
Description
Technical field
Present invention relates particularly to a kind of desalination bleaching method of Lactulose liquid.
Background technology
Isomerized lactose is with two kinds of dosage forms presence, isomerized lactose powder and Lactulose liquid in the market.Different
Structure Lactose is the product being produced for raw material through isomery, decolouring, desalination, evaporation and concentration with Lactose, because isomate process needs
Add salt, thus result in electrical conductivity height in Lactulose liquid, patent cn 1324956n and patent cn1093410a adopt ion
Exchange process desalination, because Lactulose liquid electrical conductivity is high, ion exchange desalination efficiency lost resin is fast, needs frequent regeneration, and one
Aspect efficiency is low, and besides resin regeneration can consume a large amount of soda acids and produce acid-base waste fluid, not only increase production cost, also increase
Add sewage treatment load.
Patent cn102180913a carries out the desalination of lactulose liquid using Nanofiltering membrane, and patent cn1036406c adopts electric osmose
Analysis method carries out the recycling although the purpose that desalination or salt recycle also can be reached of part salt, but either nanofiltration is also
It is that electrodialysis have strict demand to the mass concentration of material, typically require mass concentration below 15%, better effects to be obtained,
Even require below 10%, this is accomplished by before processing and using substantial amounts of water, material is diluted, because finished product requires material
At least more than 70%, this is accomplished by subsequently falling a large amount of water evaporations adding mass concentration, needs to consume a large amount of steam, this is just
Considerably increase the production cost of product.
Content of the invention
In order to solve the above-mentioned problems in the prior art, the present invention is carried out using sequential type simulated moving bed chromatography method
The desalination of Lactulose liquid, can also remove partial pigment simultaneously, and remaining salinity is removed further using ion exchange, will
Electrical conductivity is down to below 15us/cm, reaches target level of product quality.
The technical solution used in the present invention is as follows:
A kind of desalination bleaching method of Lactulose liquid, comprises the following steps:
(1) the prepared Lactulose liquid of Lactose chemical isomerization is carried out desalination using sequential type simulated moving bed chromatography to take off
Color, obtains three components, respectively salt component, isomerized lactose component and colour component;
(2) by the isomerized lactose group lease making obtaining in step (1) decolouring and ion exchange resin desalination, prepared desalination takes off
Liquid isomerized lactose product after color.
Further, the salt component obtaining in step (1) is carried out as the isomery agent changed sugar water and react of Lactose
Recycling.That is, change the sugar water and the chemical isomerization agent of reaction that adopt during Lactose chemical isomerization are the salt obtaining in step (1)
Component.
In step (1), Lactose chemical isomerization adopt alkali isomerization agent, including sodium hydroxide, potassium hydroxide, calcium hydroxide,
The mixture of one or more of sodium carbonate, potassium carbonate, sodium phosphate, potassium phosphate, sodium phosphite, potassium phosphite etc..
The separating medium that described sequential type simulated moving bed chromatography adopts is na+、ca2+、k+In type cation exchange resin
One kind, wherein from the point of view of final desalination bleaching effect, preferably sodium form cation exchange resin.
Wherein, the change adopting when the ion-type of separating medium that sequential type simulated moving bed chromatography is selected is with Lactose chemical isomerization
The ion-type learning isomery agent is identical.
In order to not affect separating effect, the ion-type of the separating medium that sequential type simulated moving bed chromatography is selected must be with chemistry
The ion-type of isomery agent is identical, and such as, chemical isomerization agent selects sodium hydroxide and/or sodium carbonate and/or sodium phosphate and/or phosphorous
The isomery agent containing sodium ion such as sour sodium, then separating medium selects sodium form cation exchange resin;Chemical isomerization agent selects hydrogen-oxygen
Change the isomery agent containing potassium ion such as potassium, then separating medium selects potassium type cation exchange resin.Select the carried cation of resin
The reason need identical with the cation containing in Lactulose liquid is to prevent from causing resin cation in running by thing
Cation in material replaces, and causes ion exchange resin conversion, affects separating effect.
The method of sequential type simulated moving bed chromatography separation isomerized lactose in the present invention, to the mass concentration of material not
It is particularly limited to, it is contemplated that for separating effect and separation efficiency and cost, entering as sequential type simulated moving bed chromatography
The Lactulose liquid mass concentration of material is preferably 45-55%;The ph of its feedstock solution is 4-8.This Lactulose liquid is in matter
Electrical conductivity during amount concentration 20% is 8000-9000us/cm, and light transmittance is 20-25%.
The Lactulose liquid matter that the mass concentration of sequential type simulated moving bed chromatography charging is obtained with Lactose chemical isomerization
Amount concentration is consistent to be separated it is not necessary to be adjusted compared to electrodialysis, eliminates this link of dilution, cost-effective, reduces energy
Consumption.Avoid excessive concentration meeting build-up of pressure too high, affect separating effect, concentration is too low to cause asking of low production efficiency simultaneously
Topic.
Preferably, it is 55-75 DEG C using the separation temperature of sequential type simulated moving bed chromatography.
Described sequential type simulated moving bed chromatography is made up of that (6 root chromatogram column head and the tail are composed in series simulation and move 6 root chromatogram columns
Bed chromatographic separation device, separating medium is filled in chromatographic column), on off state is controlled by electromagnetic valve, feed, discharging and
Circulation is all interval;Further, each cycle is made up of three steps, and first walks out of salt component and colour component, and the time is
302s, second step is isomerized lactose component, and the time is 440s, and the 3rd step is circulation time, and the time is 780s.
Preferably, the particle diameter of the separating medium that described sequential type simulated moving bed chromatography adopts is 0.25-0.35mm, described point
It is that granule is uniform, the homogeneous microsphere in aperture from the resin of agent, coefficient of uniformity is less than 1.5, preferably smaller than 1.1.
The separating medium that described sequential type simulated moving bed chromatography adopts, with acid macroporous resin as carrier, is chelated gold
Belong to ion, using cross-linking agent by metal ion-chelant on macroporous resin, weight/mass percentage composition in macroporous resin for the cross-linking agent
For 6-14%.
For sequential simulated moving bed operating parameter, such as chromatograph column volume, the flow velocity of eluting water, feed flow rate,
Rate of circulating flow, tapping flowrate of salt component, isomerized lactose component and colour component etc., different with the difference of scale, according to
Practical situation carries out selecting adjustment, and right there is no particular requirement that.
After sequential type simulated moving bed chromatography separates, the mass concentration of described isomerized lactose component is 23-28%;
Electrical conductivity is 900-1100us/cm;Light transmittance is 70-75%.Described electrical conductivity and light transmittance are isomerized lactose group sub-prime
Amount concentration is to measure when 20%.
In step (2), the decolouring further of isomerized lactose component adopts activated carbon decolorizing, and activated carbon dosage is about to live
Property carbonaceous amount: solid quality=1:80~90 in Lactulose liquid, without sequential type simulated moving bed chromatography desalination bleaching
The same efficacy activities charcoal consumption that reaches be about quality of activated carbon: solid quality=1:35 in Lactulose liquid, live
The consumption of property charcoal has saved 1/2~2/3.After adopting activated carbon decolorizing further, the pigment in material is substantially all taken off
Remove.
Described ion exchange resin includes cation exchange resin and anion exchange resin, wherein anion exchange resin
For weak-base anion-exchange resin, material electrical conductivity is down to below 15us/cm (isomerized lactose group sub-prime after ion exchange
Amount concentration is to measure when 20%).Anion exchange resin easily causes material component using strong-base anion-exchange resin
Change, therefore only allows to adopt weak-base anion-exchange resin.
The present invention also provides the liquid isomery that a kind of desalination bleaching method using above-mentioned Lactulose liquid prepares
Change lactose prod.This product isomerized lactose constituent mass concentration be 20% when, measure its electrical conductivity be down to 15us/cm with
Under, illustrate that the salt impurity in this product has been obtained for sufficiently removing;And the pigment in this product is substantially also whole
Removing.
This product also can concentrate the liquid isomerized lactose product after preparing concentration further.
Simulated moving bed chromatography is a kind of modernization separation equipment, and it is combined with suitable adsorption separating agent, can efficiently,
Separate many conventional methods at a low price and be difficult to detached material.Therefore, on modern industry, food, change have been largely used to it
Product are separated with pharmaceuticals.The principle of simulated moving bed chromatography, is to the different component adsorptivity in liquid phase using adsorbent
Different component in liquid phase, using the cyclic program of absorption, eluting, is continuously separated by the difference of energy.This technique is big at present
Measure for petrochemical industry and food industry.On the basis of simulated moving bed chromatography, in recent years, created sequential simulated movement
Bed chromatograph, sequential type simulated moving bed chromatography is with the difference of simulated moving bed chromatography, chromatographic column consumption is few, and separating effect is more
Good, a step of simulated moving bed chromatography is divided into two or multistep, charging and discharging and circulation are intervals, therefore not only save
About invest, and the product purity obtaining is higher.
The present invention carries out the key point of the desalination bleaching of Lactulose liquid first using sequential type simulated moving bed chromatography
It is suitable separating medium, the besides compound mode of chromatographic column, each including water inlet, charging, salinity, isomerized lactose and pigment
The charging of component and the relative position of discharging, are finally operating parameters, and suitable separating medium is to ensure that the premise of separating effect.
One of technique scheme technical scheme has the advantages that
(1) carrying out desalination bleaching using sequential type simulated moving bed chromatography method is that those skilled in the art does not allow to be readily conceivable that
, reason is: has a strict demand to the electrical conductivity of sequential type simulated moving bed chromatography method charging in prior art: typically require into
Expect electrical conductivity in below 50us/cm, so not allowing to be readily conceivable that the desalination carrying out material using sequential type simulated moving bed chromatography method,
This technology carries out desalination using sequential type simulated moving bed chromatography method, strict requirements have been done to the ion-type of separating medium it is desirable to
It must be identical with the ion-type containing in Lactulose liquid.
Carry out the desalination of Lactulose liquid using sequential type simulated moving bed chromatography method, salt rejection rate reaches more than 85%,
It is to solve fast, the frequent regeneration that lost efficacy only with ion exchange desalination ion exchange resin, the low problem of efficiency first;Again
It is a large amount of soda acids having saved ion exchange resin regeneration consumption, reduce the generation of acid-base waste fluid simultaneously, saved and produced into
Basis and cost of sewage disposal;Separating medium resin used is repeatable utilization, and resin life, up to 5-8, greatly reduces and runs
Cost.
(2) carry out the desalination of Lactulose liquid using sequential type simulated moving bed chromatography method, solve NF membrane simultaneously
Method and electroosmose process desalination need to add water to dilute material, need to consume the present situation of a large amount of steam, are the life of Lactulose liquid
Produce the production method providing a kind of economy.
(3) the salt component that sequential type simulated moving bed chromatography method of the present invention obtains, the change sugar water as Lactose and reaction
Isomery agent recycling, not only saved the cost of isomery agent, decrease Lactulose liquid production process waste liquid row
Put, make entirely to produce more safety and environmental protection.
(4) carry out the desalination of Lactulose liquid using sequential type simulated moving bed chromatography method, while solving desalination
The color of material has been carried out most removing, has achieved the effect of decolouring simultaneously, this be originally it is not expected that.
Brief description
Fig. 1, Fig. 2 and Fig. 3 represent three steps in sequential type simulated moving bed chromatography method desalination bleaching a cycle
Schematic diagram, after this periodic duty is complete, all running statuses switch to next chromatographic column, by that analogy, wherein No. 6 chromatographic columns
Next chromatographic column is No. 1 chromatographic column.The 1 of in figure represents No. 1 chromatographic column, 2 represents No. 2 chromatographic columns, 3 represents No. 3 chromatographic columns, 4 generations
No. 4 chromatographic columns of table, 5 represent No. 5 chromatographic columns, 6 represent No. 6 chromatographic columns.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
Mass concentration is 50%, ph be 7.5 Lactulose liquid as 10l (cumulative volumes of 6 root chromatogram columns) sequentially
The charging of formula simulated moving bed chromatography, this quality of material concentration is electrical conductivity when 20% is 8790us/cm, and light transmittance is
22%, feed flow rate is 50ml/min, and water inlet flow velocity is 46ml/min, and rate of circulating flow is 47ml/min, when temperature is 65 DEG C
Carry out desalination, obtain salt component, isomerized lactose component and colour component, the mass concentration of wherein Lactulose liquid component is
26%, mass concentration is electrical conductivity when 20% is 960us/cm, and light transmittance is 75%, by it through activated carbon decolorizing (activated carbon
Consumption be quality of activated carbon: solid quality=1:90 in Lactulose liquid), ion exchange resin desalination and evaporation and concentration
After obtain isomerized lactose finished product, salt component as Lactose change sugar water and react isomery agent reuse, colour component
Enter sewage plant.
The isomery agent adopting during Lactose chemical isomerization in the present embodiment is sodium hydroxide, accordingly, sequential simulated movement
The separating medium that bed chromatograph adopts is sodium form cation exchange resin, and its particle diameter is 0.25-0.35mm, and coefficient of uniformity is less than 1.1, hands over
Connection weight/mass percentage composition in macroporous resin for the agent is 8%.
Described ion exchange resin includes cation exchange resin and anion exchange resin, wherein anion exchange resin
For weak-base anion-exchange resin.
Described sequential type simulated moving bed chromatography is made up of that (6 root chromatogram column head and the tail are composed in series simulation and move 6 root chromatogram columns
Bed chromatographic separation device, separating medium is filled in chromatographic column), on off state is controlled by electromagnetic valve, feed, discharging and
Circulation is all interval, and each cycle is made up of three steps, and first walks out of salt component and colour component, and the time is 302s, second step
For going out isomerized lactose component, the time is 440s, and the 3rd step is circulation time, and the time is 780s.
Fig. 1, Fig. 2 and Fig. 3 represent three steps in sequential type simulated moving bed chromatography method desalination bleaching a cycle,
After this periodic duty is complete, all running statuses switch to next chromatographic column, by that analogy, next chromatograph of wherein No. 6 chromatographic columns
Post is No. 1 chromatographic column.
Fig. 1 illustrates: colour component is collected in No. 2 chromatographic column import water inlets, outlets, and No. 5 chromatographic column inlet feed, outlets connect
No. 6 chromatographic column imports, No. 6 column outlet collect salinity component, and No. 1 chromatographic column, No. 3 chromatographic columns and No. 4 chromatographic columns are now stopped
Only run.
Fig. 2 illustrates: No. 2 chromatographic column import water inlets, No. 2 column outlet connect No. 3 chromatographic column imports, No. 3 chromatographic columns and go out
Mouth connects No. 4 chromatographic column imports, No. 4 column outlet connect No. 5 chromatographic column imports, No. 5 column outlet No. 6 chromatographic columns of connection
Import, No. 6 column outlet collect isomerized lactose component.
Fig. 3 illustrates: No. 1 column outlet No. 2 chromatographic column imports of connection, No. 2 column outlet connect No. 3 chromatographic columns and enter
Mouth, No. 3 column outlet No. 4 chromatographic column imports of connection, No. 4 column outlet connect No. 5 chromatographic column imports, No. 5 chromatographic columns and go out
Mouth connects No. 6 chromatographic column imports, No. 6 column outlet connect No. 1 chromatographic column imports.
Measure when isomerized lactose constituent mass concentration is 20%, material electrical conductivity is down to 6.4us/ after ion exchange
Cm about.
Embodiment 2
Mass concentration is 45%, ph be 4 Lactulose liquid as 10l (cumulative volumes of 6 root chromatogram columns) sequential
The charging of simulated moving bed chromatography, particular order formula simulated moving bed chromatography program as described in Example 1, this quality of material concentration
It is 8545us/cm for electrical conductivity when 20%, light transmittance is 24%, feed flow rate is 56ml/min, water inlet flow velocity is 52ml/
Min, rate of circulating flow is 53ml/min, carries out desalination when temperature is 55 DEG C, obtains salt component, isomerized lactose component and pigment
Component, the wherein mass concentration of Lactulose liquid component are 23%, and mass concentration is electrical conductivity when 20% is 943us/cm,
Light transmittance is 73%, and by it, through activated carbon decolorizing, (consumption of activated carbon is quality of activated carbon: solid material in Lactulose liquid
Amount=1:85), obtain isomerized lactose finished product after ion exchange resin desalination and evaporation and concentration, salt component is as the change sugar of Lactose
Reused with the isomery agent of water and reaction, colour component enters sewage plant.
The isomery agent adopting during Lactose chemical isomerization in the present embodiment is potassium carbonate, accordingly, sequential simulated moving bed
The separating medium that chromatograph adopts is potassium type cation exchange resin, and its particle diameter is 0.25-0.35mm, and coefficient of uniformity is less than 1.1, crosslinking
Weight/mass percentage composition in macroporous resin for the agent is 10%.
Described ion exchange resin includes cation exchange resin and anion exchange resin, wherein anion exchange resin
For weak-base anion-exchange resin.
Measure when isomerized lactose constituent mass concentration is 20%, material electrical conductivity is down to after ion exchange
10.6us/cm about.
Embodiment 3
Mass concentration is 55%, ph be 8 Lactulose liquid as 10l (cumulative volumes of 6 root chromatogram columns) sequential
The charging of simulated moving bed chromatography, particular order formula simulated moving bed chromatography program as described in Example 1, this quality of material concentration
It is 8312us/cm for electrical conductivity when 20%, light transmittance is 22%, feed flow rate is 46ml/min, water inlet flow velocity is 46ml/
Min, rate of circulating flow is 46ml/min, carries out desalination when temperature is 75 DEG C, obtains salt component, isomerized lactose component and pigment
Component, the wherein mass concentration of Lactulose liquid component are 27.5%, and mass concentration is electrical conductivity when 20% is 1064us/
Cm, light transmittance is 71%, and by it, through activated carbon decolorizing, (consumption of activated carbon is quality of activated carbon: solid in Lactulose liquid
Amount of substance=1:83), obtain isomerized lactose finished product after ion exchange resin desalination and evaporation and concentration, salt component is as Lactose
Change the isomery agent recycling of sugar water and reaction, colour component enters sewage plant.
The isomery agent adopting during Lactose chemical isomerization in the present embodiment is calcium hydroxide, accordingly, sequential simulated movement
The separating medium that bed chromatograph adopts is ca2+Type cation exchange resin, its particle diameter is 0.25-0.35mm, and coefficient of uniformity is less than 1.1,
Weight/mass percentage composition in macroporous resin for the cross-linking agent is 12%.
Described ion exchange resin includes cation exchange resin and anion exchange resin, wherein anion exchange resin
For weak-base anion-exchange resin.
Measure when isomerized lactose constituent mass concentration is 20%, material electrical conductivity is down to 8.1us/ after ion exchange
Cm about.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-described embodiment
Limit, other any spirit without departing from the present invention and the change made under principle, modification, replacement, combine, simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (10)
1. a kind of desalination bleaching method of Lactulose liquid, is characterized in that, comprise the following steps:
(1) Lactulose liquid that Lactose chemical isomerization is obtained carries out desalination bleaching using sequential type simulated moving bed chromatography,
Obtain three components, respectively salt component, isomerized lactose component and colour component;
(2) by the isomerized lactose group lease making obtaining in step (1) decolouring and ion exchange resin desalination, prepared desalination bleaching liquid
Body isomerized lactose product.
2. desalination bleaching method as claimed in claim 1, is characterized in that: using the salt component obtaining in step (1) as Lactose
Change sugar with water and reaction isomery agent reused.
3. desalination bleaching method as claimed in claim 1, is characterized in that: in step (1), Lactose chemical isomerization is different using alkalescence
Structure agent, including sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, potassium carbonate, sodium phosphate, potassium phosphate, sodium phosphite, phosphorous
The mixture of one or more of sour potassium.
4. desalination bleaching method as claimed in claim 1, is characterized in that: in step (1), described sequential simulated moving bed color
The separating medium that spectrum adopts is na+、ca2+、k+One of type cation exchange resin, wherein, sequential type simulated moving bed chromatography
From separating medium ion-type with Lactose chemical isomerization when the ion-type of chemical isomerization agent that adopts identical.
5. desalination bleaching method as claimed in claim 4, is characterized in that: described separating medium is sodium form cation exchange resin.
6. desalination bleaching method as claimed in claim 1, is characterized in that: in step (1), as sequential simulated moving bed color
The Lactulose liquid mass concentration of spectrum charging is 45-55%, ph4-8, electrical conductivity 8000-9000us/cm, and light transmittance is 20-
25%.
7. desalination bleaching method as claimed in claim 1, is characterized in that: in step (1), using sequential simulated moving bed color
The separation temperature of spectrum is 55-75 DEG C.
8. desalination bleaching method as claimed in claim 1, is characterized in that: in step (1), described sequential simulated moving bed color
Spectrum is made up of 6 root chromatogram columns, and on off state is controlled by electromagnetic valve, and charging, discharging and circulation are all intervals;Preferably
, each cycle is made up of three steps, and first walks out of salt component and colour component, and the time is 302s, and second step is isomerization breast
Saccharic composition, the time is 440s, and the 3rd step is circulation time, and the time is 780s.
9. desalination bleaching method as claimed in claim 1, is characterized in that: in step (1), described sequential simulated moving bed color
The particle diameter of the separating medium that spectrum adopts is 0.25-0.35mm, and coefficient of uniformity is less than 1.5, and preferably coefficient of uniformity is less than 1.1;
In step (2), decolouring adopts activated carbon decolorizing;Described ion exchange resin includes cation exchange resin and anion is handed over
Change resin, wherein anion exchange resin is weak-base anion-exchange resin, and material electrical conductivity is down to after ion exchange
Below 15us/cm.
10. the liquid being prepared using the desalination bleaching method of the Lactulose liquid any one of claim 1~9
Isomerized lactose product.
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CN110368716A (en) * | 2019-07-31 | 2019-10-25 | 赛普特环保技术(厦门)有限公司 | A kind of sugar, inorganic salts separation system and method |
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CN108997259A (en) * | 2018-08-31 | 2018-12-14 | 山东亚邦化工科技有限公司 | The technique and device decolourized for synthetic sweetener acesulfame potassium or mother liquor of sucralose |
CN109646999A (en) * | 2018-11-23 | 2019-04-19 | 吉林中粮生化有限公司 | It is a kind of for separating the Simulation moving bed and method of glucide |
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CN110368716B (en) * | 2019-07-31 | 2023-11-14 | 赛普特环保技术(厦门)有限公司 | Sugar and inorganic salt separation system and method |
CN113893578A (en) * | 2021-09-08 | 2022-01-07 | 四川雅华生物有限公司 | Separation and purification system and process method of hydrolysate |
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