CN107840782A - The production method and device of sorbierite - Google Patents
The production method and device of sorbierite Download PDFInfo
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- CN107840782A CN107840782A CN201710953369.8A CN201710953369A CN107840782A CN 107840782 A CN107840782 A CN 107840782A CN 201710953369 A CN201710953369 A CN 201710953369A CN 107840782 A CN107840782 A CN 107840782A
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses the production method of ultra-high purity sorbierite, its step are as follows:Starch saccharificating liquid is decolourized, obtains Sorbitol solution from hydrogenation after friendship, Sorbitol solution obtains coarse filtration Sorbitol solution after filtering;Enter sorbierite cleaner liquid and concentrate that membranous system is filtrated to get high-purity after the cooling of coarse filtration Sorbitol solution, sorbierite cleaner liquid purity is between 95~97%;High-purity sorbierite cleaner liquid obtains ultra-high purity Sorbitol solution after decolourizing again, and purity is 98~99.5%;Ultra-high purity Sorbitol solution is concentrated or condensing crystallizing after obtain ultra pure liquids sorbierite or crystalline sorbitol.Advantage of the present invention:Using membrane separation technique to Sorbitol solution separating-purifying, separating obtained sorbierite cleaner liquid purity is high, quality better, through decolourizing again, from friendship after obtain the Sorbitol solution that ultra-high purity obtains, film concentrate can make maltitol product and sell, realize raw material 100% utilize.
Description
Technical field
The present invention relates to the production field of sugar alcohol, is a kind of producer that ultra-high purity sorbierite is produced using membrane technology
Method.
Background technology
Sorbierite is widely used fine chemicals, is widely used in all multirows such as medicine, food, cosmetics, tobacco
In industry, different industries are different to sorbierite quality requirements standard.The preparation method of sorbierite has catalytic hydrogenation method, electricity at present
Solve reducing process, biological fermentation process.For requiring the not high technical grade product sorbierite of purity to preparation, catalytic hydrogenation method has preparation
The advantage that method method is simple, cost is low, but the use of catalytic hydrogenation method catalyst type is limited to, the purity of product needs
Improve.
In patent of invention CN10515447A, inventor by starch successively through liquefying, being saccharified, cleaning, decolouring desalination, receive
The process condensing crystallizings such as filter purification, film concentration, evaporation and concentration, hydrogenation, continuous ionic film desalination and concentration obtain sorbierite, this production
Method complex technical process, equipment investment cost are high, require high to equipment and technology, and the economic utilization of the energy is unreasonable, it is difficult to general
All over realizing industrialized production.
The content of the invention
To improve sorbierite purity and reducing production cost, simplified technological operation, the present invention is separated using membrane separation technique
Monose alcohol and polysaccharide polyol, and then produce ultra-high purity sorbierite;Alcohol liquid after hydrogenation catalyst can obtain 95% after membranous system separates
~97% sorbierite cleaner liquid;Clear liquid decolourizes through film again, from sequence of handing over after the sorbierite of ultra-high purity can be made;Film trapped fluid can
Make the sale of high added value maltitol, realize that raw material 100% utilizes.
It is an object of the invention to provide the production method of ultra-high purity sorbierite, produces ultra-high purity sorbierite, solves to use
The problem of catalytic hydrogenation conventional method product quality is poor, purity is low.Film concentrate is alternatively arranged as the malt of another high added value
Sugar alcohol product.
To achieve these goals, the present invention uses following scheme:
The first aspect of the invention, there is provided:
The production method of sorbierite, comprises the following steps:
1st step, hydrogenation catalyst reaction is carried out to starch saccharificating liquid, sorbierite reaction solution is prepared;
2nd step, sorbierite reaction solution is handled using the method for UF membrane, sorbierite is passed through seperation film, glycocalix seperation film
Retention.
In one embodiment, using the seperation film that molecular cut off is 200~5000Da in the method for UF membrane.
In one embodiment, seperation film is organic film.
In one embodiment, 15~55 DEG C of feed temperature, preferably 40~50 DEG C in the method for UF membrane.
In one embodiment, 1~3MPa of filter pressure in the method for UF membrane, 7~25.5L/h of membrane flux m2.
In one embodiment, sorbitol concentration 95~97% in permeate in the method for UF membrane.
In one embodiment, before the 2nd step carries out UF membrane, pre-filtering is carried out to sorbierite reaction solution.
In one embodiment, the average pore size for the filter that pre-filtering uses is less than 5 μm.
In one embodiment, before pre-filtering, the temperature of sorbierite reaction solution is cooled to 15~55 DEG C, preferably
40~50 DEG C.
In one embodiment, it is necessary to be decolourized to saccharified liquid and desalting processing before the hydrogenation catalyst of the 1st step.
In one embodiment, decolorization process is to use activated carbon decolorizing, and bleaching temperature is at 60~80 DEG C, decolorization material
Liquid pH4.0~4.2, decolouring number are 1~2 time;Feed liquid light transmittance >=99% after decolouring.
In one embodiment, desalting steps are taken off using male post exchanger resin and/or anion column exchanger resin
Salt.
In one embodiment, pH4.2~4.4 when starch saccharificating liquid enters in desalting steps, 40~50 DEG C of temperature, concentration
Concentration of glucose 45~50%.
In one embodiment, 120~140 DEG C of the reaction temperature of hydrogenation catalyst reaction, 10~14Mpa of pressure.
In one embodiment, the sorbierite permeate of the seperation film obtained in the 2nd step passes through decolorization.
In one embodiment, decolorization is to use activated carbon decolorizing, and bleaching temperature is at 60~80 DEG C, decolorization material
Liquid pH4.0~4.2, decolouring number are 1~2 time.
In one embodiment, the sorbierite permeate after decolorization is needed by concentration.
In one embodiment, described concentration concentrate, be spray-dried selected from film, be concentrated under reduced pressure in one kind.
In one embodiment, after sorbierite permeate concentration sorbierite purity 98~99.5%.
The second aspect of the invention, there is provided:
The process units of sorbierite, including:
Hydrogenation reaction kettle, for carrying out hydrogenation reaction to starch saccharificating liquid;
Seperation film, hydrogenation reaction kettle is connected to, for carrying out UF membrane to reaction product, sorbierite is passed through seperation film, polysaccharide
Be separated film retention.
In one embodiment, the molecular cut off of seperation film is 200~5000Da.
In one embodiment, seperation film is organic film.
In one embodiment, in addition to the first decoloring reaction kettle, for carrying out decolorization to starch saccharificating liquid;Also wrap
Ion exchange resin column is included, starch saccharificating liquid carries out desalting processing;The material liquid outlet of first decoloring reaction kettle passes through ion exchange
Resin is connected to the liquor inlet of hydrogenation reaction kettle.
In one embodiment, in addition to prefilter, hydrogenation reaction kettle is connected to, for the reaction to entering seperation film
Product carries out pre-filtering.
In one embodiment, in addition to the first enrichment facility and the second enrichment facility;First enrichment facility is connected to point
From the retention side of film, for carrying out concentration to trapped fluid;Second enrichment facility is connected to the per-meate side of seperation film, for pair
Penetrating fluid carries out concentration.
In one embodiment, in addition to the second decoloring reaction kettle, the per-meate side of seperation film is connected to, for penetrating fluid
Carry out concentration.
In one embodiment, it is dense to be selected from evaporation concentration device, film for the first described enrichment facility and the second enrichment facility
One kind in compression apparatus or spray-drying installation.
In one embodiment, activated carbon is set to add part on the first decoloring reaction kettle and the second decoloring reaction kettle.
Beneficial effect
Technique of the present invention has the following advantages:
(1)The sorbierite cleaner liquid isolated is crossed after membranous system, and purity obtains ultra-high purity up to 95~97% after decolourizing from friendship
Sorbierite, raw material availability is high, and loss is few, and sorbierite output capacity is high.
(2)The concentrate maltitol purity that film is concentrated to give is high, can make maltitol product utilization.
(3)Ultra-high purity sorbierite is produced with membrane separation process, substantially increases product purity, energy consumption is reduced and is produced into
This.
Brief description of the drawings
Fig. 1 is sorbierite production method flow chart provided by the invention;
Fig. 2 is sorbierite production method installation drawing provided by the invention;
Wherein, the 1, first decoloring reaction kettle;2nd, ion exchange resin column;3rd, hydrogenation reaction kettle;4th, prefilter;5th, seperation film;
6th, the first enrichment facility;7th, the second decoloring reaction kettle;8th, the second enrichment facility.
Embodiment
The present invention is described in further detail below by embodiment combination accompanying drawing.But those skilled in the art
It will be understood that the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.It is unreceipted in embodiment
Particular technique or condition person, (such as write according to the technology described by document in the art or condition with reference to Xu Nan equalitys
《Inorganic membrane separation technique and application》, Chemical Industry Press, 2003) or carry out according to product description.Agents useful for same or
The unreceipted production firm person of instrument, being can be by the conventional products of acquisition purchased in market.
Approximate language used herein can be used for modifying any quantity statement in entire disclosure and claims, and it can
Permit being changed under conditions of the basic function for not causing its related changes.Therefore, repaiied by term such as " about "
The value of decorations is not limited to specified exact value.In at least some cases, approximate language can be with the instrument for measuring the value
Precision it is corresponding.Unless being indicated otherwise in context or sentence, otherwise range limit can be combined and/or exchange, and
And this scope is confirmed as and including all subranges contained herein.Except in embodiment is operated or elsewhere
In indicate outside, the numeral of the amounts of all expression compositions used in specification and claims, reaction condition etc. or
Expression shall be construed as the modification by word " about " in all cases.Heretofore described percentage is especially said in nothing
All referring to mass percent in the case of bright.
The invention provides a kind of method and device for producing sorbierite, has higher product purity.
Raw material of the present invention is starch saccharificating liquid.
In the present invention, term " starch " refers to any material being made up of the complicated polysaccharide carbohydrate of plant, including
With formula (C6H10O5) x amylose and amylopectin, wherein x can be any number.The source of starch includes cereal
And/or the vegetable material comprising granular starch.Vegetable material available from plant, including but not limited to wheat, corn, rye,
Sorghum(Chinese sorghum), rice, grain, barley, triticale, cassava(Cassava), potato, sweet potato, beet, sugarcane and such as soybean and pea
Beans.The available vegetable material of the present invention includes corn, barley, wheat, rice, sorghum and combinations of the above.Vegetable material can
Including hybridization mutation and genetic modification mutation(Such as include transgenic corns, barley or the soybean of heterologous gene).Plant it is any
Part can be used in providing substrate, including but not limited to plant part, for example, leaf, stem, crust, shell, stem tuber, corncob,
Grain etc..In some embodiments, substantially whole plant can be used, for example, intact corn stalk can be used.One
In a little embodiments, whole grain can be used as the source of granular starch.Whole grain includes corn, wheat, rye, barley, height
Beam and combinations of the above.In other embodiments, the cereal grains that granular starch separates available from classification, including fiber, embryo
Breast and/or plumule composition.In some embodiments, the starch of separate sources can be mixed to obtain in the inventive method
The raw material used(Such as corn and chinese sorghum or corn and barley).
In some embodiments, starch is to be prepared by vegetable material by modes such as crushing.Such as pass through grinding(Sledge mill
Or roller mill), emulsifying technology, rotary pulse, the mode such as fractionation obtain the granularity of suitable starch.
Next, needing to be prepared as slurry to starch, " dry solid content " is by the total solid in slurry(Represented with %),
Calculated based on dry weight.In some embodiments, it is mutually mixed as slurry with water and granular starch, can be wrapped in slurry
About 10%~55% dry solid content is included, either about 25%~45% dry solid content or about 30%~35% dry solid content.
, it is necessary to be liquefied to it after starch size is obtained, liquefied effect is to make starch size that part occur
Hydrolysis, exposing more can be by non-the redeeming a vow to a god property end of saccharification enzyme effect, while viscosity declines, and mobility enhancing, is carbohydrase
Effect provide advantage.The liquifying method of the starch size can be divided into acid system or enzyme according to the difference of hydrolysis power
Method, the difference according to production technology can be divided into batch (-type), semi continuous or continous way, and the difference according to liquefaction device can be with
It is divided into tubular type, pot type or injecting type.In practical application there is crossover phenomenon in species method, such as intermittent warming treatment liquefaction process, continuously
Spray liquefaction process etc..
After liquid starchy slurry has been obtained, alpha-amylase therein can be carried out at enzyme deactivation by way of conventional
Reason, such as handled at a high temperature of 100~150 DEG C., it is necessary to which to add carbohydrase further by its after liquefying starch has been obtained
Ground is hydrolyzed, and in the present invention, " carbohydrase " and " glucoamylase " refers to the enzyme of amyloglucosidase enzyme(E.C.3.2.1.3, Portugal
Saccharogenic amylase, α-Isosorbide-5-Nitrae-D- glucan glucohydralases).These are the enzymes of circumscribed effect, and it is from amylose and amylopectin
The non-reducing end release glucose residue of molecule, these enzymes also can be with relatively low speed hydrolyzing alpha -1,6 key and α -1,3 keys.Saccharification
Enzyme is typically selected:Fungal amylase, beta amylase, glucose turn glycosides enzyme etc..Saccharifying can typically continue 6~120 hours,
Preferably 12~72 hours in the present invention, common saccharification temperature is in the lower progress of 30~65 DEG C of temperature and pH4.0~5.0.
In addition during liquefaction and saccharification, other enzymes can also be optionally included in the enzyme of addition.Other enzymes can
Including but not limited to:Cellulase, hemicellulase, zytase, protease, phytase, amylopectase, p- amylase,
Lipase, cutinase, pectase, D. dextranases, p- glucosidases, galactosidase, esterase, cyclodextrin turn glycosyl transferase
In one or several kinds of combinations.
In one embodiment, after starch saccharificating liquid has been obtained, conventional discoloration method can be used to enter it
Row decolorization, activated carbon decolorizing is preferably used here, can generally use and activated carbon is added in feed liquid, at a certain temperature
Heating response is carried out to be decolourized, the addition of activated carbon can be the 1~30% of starch saccharificating liquid weight here, e.g. 5%,
10%、15%、20%、25%;Reaction temperature can be 15~85 DEG C, such as:20℃、25℃、30℃、35℃、40℃、45℃、50
℃、55℃、60℃、65℃、70℃、75℃、80℃.Decolouring number can be 1~5 time, after decolorization, the light transmittance of feed liquid
>=99% can be reached.
In one embodiment, after being decolourized to starch saccharificating liquid, it can be carried out using ion exchange resin
Desalting processing.Here ion exchange resin (such as cationic ion-exchange resin and anion exchange resin) is used as column material
The removal of the salinity of saccharified liquid can be carried out realizing.Cationic ion-exchange resin include strong-acid cation-exchange resin and weak acid sun from
Sub-exchange resin.Strong-acid cation-exchange resin can be unit price or multivalent metal cation form, such as H+、Mg2+、Ca2+、
Sr2+Or Zn2+Form.Strong-acid cation-exchange resin generally has styrene skeleton, its preferably with 3~8%, preferably 5~6.5%
Divinyl benzene crosslinked.Weak-acid cation exchange resin can be monovalence or multivalent metal cation form, such as H+、Mg2+、
Ca2+、Sr2+Form or Na+Form.
After the starch saccharificating liquid after having obtained desalting processing, mountain can be translated into by way of hydrogenation catalyst
Pears alcohol, 120~140 DEG C of hydrogenation catalyst process reaction temperature here, 10~14Mpa of pressure.
After hydrogenation reaction, the larger granule foreign in feed liquid can be removed in a manner of coarse filtration, as
Filter type, band filter, belt press, flypress, precoat filter, filter press, the prefilter of use can be illustrated
The average pore size of filter medium be preferably smaller than 5 μm.
After pre-filtering has been carried out, filtration treatment is carried out to feed liquid using organic separation membrane, due to after reacting
Feed liquid in addition to containing sorbierite, also containing some polysaccharide(Mainly maltose), present invention discover that using retention point
Son amount can effectively make sorbierite pass through the transmission that film layer obtains mainly containing sorbierite for 200~5000Da seperation film
Liquid, and maltitol can be trapped, and then realize the separation to sorbierite and maltitol, can obtain purity compared with
High sorbierite, while the maltitol in trapped fluid can also recycle again.The material of seperation film can use acetic acid
The macromolecule material such as cellulose-based polymer, polyamide, SPSF, polyacrylonitrile, polyester, polyimides and polyvinyl
Material.
After sorbierite permeate has been obtained, can equally the method for activated carbon decolorizing be used to carry out at decolouring it
Reason.
For permeate and concentrate, it can be concentrated product by the way of concentration.
In some preferable technological parameters, technique of the present invention, step(6)Described film is that molecular cut off is
200~5000Da organic film, membrane filtration pressure are 1~3MPa, and it is 40~42 DEG C that Sorbitol solution, which enters film temperature, film device temperature
Meter shows filtration temperature:40~50 DEG C.Before not being diluted with water toward concentrate, membrane flux gradually drops in 4~7L/h m2
Low, after cycles of concentration is up to 5 times, membrane flux gradually increases in 6~14L/h m2 sections.Inventor's discovery, material purity
Between 79~89%, filter liquor sorbierite purity is between 95%~97% after film concentrates 5 times;Wherein mountain after concentrate is dried
Pears alcohol purity is between 50~60%, and maltose purity is between 20~25%;After 5 times of concentration, doubled volume of water toward concentrate
During dilution, sorbierite purity drops to 50% or so after final dope is dried;When adding about 2 times of volume of water, final dope sorbierite
Purity drops to 40% or so;Sorbierite purity drops to 30% or so when adding about 3 times of dope volumes, and maltitol purity is left 45%
It is right.
Based on above-mentioned method, device provided by the invention is as shown in Figure 2.
The process units of sorbierite, including:
Hydrogenation reaction kettle 3, for carrying out hydrogenation reaction to starch saccharificating liquid;
Seperation film 5, hydrogenation reaction kettle 3 is connected to, for carrying out UF membrane to reaction product, sorbierite is passed through seperation film, it is more
The separated film retention of sugar.
In one embodiment, the molecular cut off of seperation film 5 is 200~5000Da.
In one embodiment, seperation film 5 is organic film.
In one embodiment, in addition to the first decoloring reaction kettle 1, for carrying out decolorization to starch saccharificating liquid;Also
Including ion exchange resin column 2, starch saccharificating liquid carries out desalting processing;The material liquid outlet of first decoloring reaction kettle 1 passes through ion
Exchanger resin 2 is connected to the liquor inlet of hydrogenation reaction kettle 3.
In one embodiment, in addition to prefilter 4, hydrogenation reaction kettle 3 is connected to, for entering seperation film 5
Reaction product carries out pre-filtering.
In one embodiment, in addition to the first enrichment facility 6 and the second enrichment facility 8;First enrichment facility 6 is connected to
The retention side of seperation film 5, for carrying out concentration to trapped fluid;Second enrichment facility 8 is connected to the per-meate side of seperation film 5,
For carrying out concentration to penetrating fluid.
In one embodiment, in addition to the second decoloring reaction kettle 7, the per-meate side of seperation film 5 is connected to, for infiltration
Liquid carries out concentration.
In one embodiment, the first described enrichment facility 6 and the second enrichment facility 8 are selected from evaporation concentration device, film
One kind in enrichment facility or spray-drying installation.
In one embodiment, activated carbon is set to add part on the first decoloring reaction kettle 1 and the second decoloring reaction kettle 7.
Embodiment 1
The production method of ultra-high purity sorbierite, comprises the following steps:
(1)Decolourize:By starch saccharificating liquid activated carbon decolorizing, at 70 DEG C, pH4.0~4.2 obtain decolouring liquid glucose through secondary decolourization,
Light transmittance >=99%.
(2)From friendship:By step(1)Gained decolouring liquid glucose exchanges desalination with positive and negative ion column successively, obtains from friendship refined sugar
Liquid;Liquid glucose enters post pH4.2~4.4, temperature 45 C, concentration 46%.
(3)Hydrogenation catalyst:By step(2)The refined liquid glucose of gained carries out hydrogenation, 130 DEG C of reaction temperature, pressure
12.0MPa, obtain Sorbitol solution.
(4)Cooling:Step(3)Gained Sorbitol solution is cooled to 40 DEG C~42 DEG C.
(5)Coarse filtration:With coarse filter to step(4)Sorbitol solution carries out coarse filtration after gained cooling, obtains coarse filtration liquid, coarse filtration mistake
Filter is aperture for the filter less than 5 μm.
(6)Membrane filtration separates:By step(5)The coarse filtration liquid obtained is sent into the organic membrane system that molecular cut off is 800Da and entered
Row UF membrane purifies, and obtains sorbierite cleaner liquid and film concentrate.It is 40~42 DEG C to enter film temperature, filter pressure:2MPa, filtering
44 DEG C of temperature, after 5 times of concentration, the water for adding concentrate certain volume multiple is diluted, and extension rate refers to plus water body accumulated amount/
Concentrated liquid accumulated amount;
(7)Decolourize:By step(6)Gained Sorbitol solution obtains the Sorbitol solution of ultra-high purity after being decolourized.
(8)Concentration:Step(7)The Sorbitol solution of gained ultra-high purity is concentrated, dry after ultra-high purity sorbierite.
(9)Film concentrate utilizes:Step(6)Gained film concentrate makees the utilization of byproduct maltitol after drying.
As can be seen from the above table, method provided by the invention can prepare the sorbierite of ultra-high purity.
Embodiment 2
The production method of ultra-high purity sorbierite, comprises the following steps:
(1)Decolourize:By starch saccharificating liquid activated carbon decolorizing, at 80 DEG C, pH4.0~4.2 obtain decolouring liquid glucose through once decolourizing,
Light transmittance >=99%.
(2)From friendship:By step(1)Gained decolouring liquid glucose exchanges desalination with two groups of positive and negative ion columns, obtains from friendship refined sugar
Liquid;Liquid glucose enters post pH4.2~4.4,40 DEG C of temperature, concentration 50%.
(3)Hydrogenation catalyst:By step(2)The refined liquid glucose of gained carries out hydrogenation, 120 DEG C of reaction temperature, pressure
12.0MPa, obtain Sorbitol solution.
(4)Cooling:Step(3)Gained Sorbitol solution is cooled to 40 DEG C~42 DEG C.
(5)Coarse filtration:With coarse filter to step(4)Sorbitol solution uses aperture as the filter less than 5 μm after gained cooling
Coarse filtration, obtain coarse filtration liquid.
(6)Membrane filtration separates:By step(5)The coarse filtration liquid obtained is sent into the organic film that molecular cut off is 2000Da and carries out film
Separating-purifying, sorbierite cleaner liquid and film concentrate are obtained, enter film temperature for 40~42 DEG C, 40 DEG C of filtration temperature, concentrate 5 times
Afterwards, the water for adding the volume multiple of concentrate 3 is diluted, and extension rate refers to plus water body accumulated amount/concentrated liquid accumulated amount;
(7)Decolourize:By step(6)Gained Sorbitol solution obtains the Sorbitol solution of ultra-high purity after being decolourized.
(8)Concentration:Step(7)After the Sorbitol solution of gained ultra-high purity is concentrated ultra-high purity sorbierite.
(9)Film concentrate utilizes:Step(6)Gained film concentrate makees by-product utilization.
As can be seen from the above table, method provided by the invention can prepare the sorbierite of ultra-high purity.
Embodiment 3
The production method of ultra-high purity sorbierite, comprises the following steps:
(1)Decolourize:By starch saccharificating liquid activated carbon decolorizing, at 60 DEG C, pH4.0~4.2 obtain decolouring liquid glucose through secondary decolourization,
Light transmittance >=99%.
(2)From friendship:By step(1)Gained decolouring liquid glucose exchanges desalination with two groups of positive and negative ion columns, obtains from friendship refined sugar
Liquid;Liquid glucose enters post pH4.2~4.4,40 DEG C of temperature, concentration 45%.
(3)Hydrogenation catalyst:By step(2)The refined liquid glucose of gained carries out hydrogenation, 110 DEG C of reaction temperature, pressure
11.0MPa, obtain Sorbitol solution.
(4)Cooling:Step(3)Gained Sorbitol solution is cooled to 40 DEG C~42 DEG C.
(5)Coarse filtration:With coarse filter to step(4)Sorbitol solution uses aperture as the filter less than 5 μm after gained cooling
Coarse filtration, obtain coarse filtration liquid.
(6)Membrane filtration separates:By step(5)The coarse filtration liquid obtained is sent into organic film and carries out UF membrane purification, obtains sorbierite
Cleaner liquid and film concentrate, enter film temperature for 40~42 DEG C, filter pressure 2MPa, 40 DEG C of filtration temperature, after 5 times of concentration, add
The water of the volume multiple of concentrate 3 is diluted, and extension rate refers to plus water body accumulated amount/concentrated liquid accumulated amount;
(7)Decolourize:By step(6)Gained Sorbitol solution obtains the Sorbitol solution of ultra-high purity after being decolourized.
(8)Concentration:Step(7)After the Sorbitol solution of gained ultra-high purity is concentrated ultra-high purity sorbierite.
(9)Film concentrate utilizes:Step(6)Gained film concentrate makees by-product utilization.
As can be seen from the above table, method provided by the invention can prepare the sorbierite of ultra-high purity.
Claims (10)
1. the production method of sorbierite, it is characterised in that comprise the following steps:
1st step, hydrogenation catalyst reaction is carried out to starch saccharificating liquid, sorbierite reaction solution is prepared;
2nd step, sorbierite reaction solution is handled using the method for UF membrane, sorbierite is passed through seperation film, polysaccharide polyol is separated
Film retains.
2. the production method of sorbierite according to claim 1, it is characterised in that in the method for UF membrane using cut
Stay the seperation film that molecular weight is 200~5000Da;Seperation film is organic film;15~55 DEG C of feed temperature in the method for UF membrane,
It is preferred that 40~50 DEG C;1~3MPa of filter pressure in the method for UF membrane, 7~25.5L/h of membrane flux m2.
3. the production method of sorbierite according to claim 1, it is characterised in that mountain in permeate in the method for UF membrane
Pears determining alcohol 95~97%;Before the 2nd step carries out UF membrane, pre-filtering is carried out to sorbierite reaction solution;What pre-filtering used
The average pore size of filter is less than 5 μm;Before pre-filtering, the temperature of sorbierite reaction solution is cooled to 15~55 DEG C, it is excellent
Select 40~50 DEG C;, it is necessary to be decolourized to saccharified liquid and desalting processing before the hydrogenation catalyst of the 1st step;Decolorization process is to adopt
With activated carbon decolorizing, for bleaching temperature at 60~80 DEG C, decolorization material liquid pH 4.0~4.2, decolouring number is 1~2 time;Decolourize
Feed liquid light transmittance >=99% afterwards.
4. the production method of sorbierite according to claim 1, it is characterised in that desalting steps are to exchange tree using male post
Fat and anion column exchanger resin carry out desalination;PH4.2~4.4 when starch saccharificating liquid enters in desalting steps, temperature 40~50
DEG C, glucose 45~50%;120~140 DEG C of the reaction temperature of hydrogenation catalyst reaction, 10~14Mpa of pressure;2nd step
In the obtained sorbierite permeate of seperation film pass through decolorization;Decolorization is to use activated carbon decolorizing, and bleaching temperature exists
60~80 DEG C, decolorization material liquid pH 4.0~4.2, decolouring number is 1~2 time;Sorbierite permeate after decolorization needs
By concentration;Described concentration concentrates selected from film, is spray-dried, be concentrated under reduced pressure in one kind.
5. the production method of sorbierite according to claim 1, it is characterised in that mountain after sorbierite permeate concentration
The purity 98~99.5% of pears alcohol.
6. the process units of sorbierite, it is characterised in that including:
Hydrogenation reaction kettle(3), for carrying out hydrogenation reaction to starch saccharificating liquid;
Seperation film(5), it is connected to hydrogenation reaction kettle(3), for carrying out UF membrane to reaction product, make sorbierite through separation
Film, the separated film retention of polysaccharide polyol.
7. the process units of sorbierite according to claim 6, it is characterised in that seperation film(5)Molecular cut off be
200~5000Da;Seperation film(5)It is organic film;Also include the first decoloring reaction kettle(1), for being taken off to starch saccharificating liquid
Color processing;Also include ion exchange resin column(2), starch saccharificating liquid progress desalting processing;First decoloring reaction kettle(1)Feed liquid
Outlet passes through ion exchange resin(2)It is connected to hydrogenation reaction kettle(3)Liquor inlet.
8. the process units of sorbierite according to claim 6, it is characterised in that also including prefilter(4), it is connected to
Hydrogenation reaction kettle(3), for into seperation film(5)Reaction product carry out pre-filtering.
9. the process units of sorbierite according to claim 6, it is characterised in that also including the first enrichment facility(6)With
Second enrichment facility(8);First enrichment facility(6)It is connected to seperation film(5)Retention side, for being carried out to trapped fluid at concentration
Reason;Second enrichment facility(8)It is connected to seperation film(5)Per-meate side, for penetrating fluid carry out concentration.
10. the process units of sorbierite according to claim 6, it is characterised in that also including the second decoloring reaction kettle
(7), it is connected to seperation film(5)Per-meate side, for penetrating fluid carry out concentration;The first described enrichment facility(6)With
Second enrichment facility(8)One kind in evaporation concentration device, film condensing device or spray-drying installation;First decolourizes instead
Answer kettle(1)With the second decoloring reaction kettle(7)Upper setting activated carbon adds part;First decoloring reaction kettle(1)Decolourized with second anti-
Answer kettle(7)Upper setting activated carbon adds part.
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