CN108503506A - A kind of new process producing high pure sorbitol using chromatographic separation technology - Google Patents

A kind of new process producing high pure sorbitol using chromatographic separation technology Download PDF

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CN108503506A
CN108503506A CN201810660854.0A CN201810660854A CN108503506A CN 108503506 A CN108503506 A CN 108503506A CN 201810660854 A CN201810660854 A CN 201810660854A CN 108503506 A CN108503506 A CN 108503506A
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chromatographic separation
ion
concentration
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exchange
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王兆光
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SHANDONG TRILLION CHROMATOGRAPHY SEPARATION TECHNOLOGY Co Ltd
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SHANDONG TRILLION CHROMATOGRAPHY SEPARATION TECHNOLOGY Co Ltd
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/132Preparation 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
    • C07C29/136Preparation 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 of >C=O containing groups, e.g. —COOH
    • C07C29/14Preparation 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 of >C=O containing groups, e.g. —COOH of a —CHO group
    • C07C29/141Preparation 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 of >C=O containing groups, e.g. —COOH of a —CHO group with hydrogen or hydrogen-containing gases
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    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
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    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H3/00Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
    • C07H3/06Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
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    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00Glucose; Glucose-containing syrups
    • C13K1/06Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch

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Abstract

The application belongs to the processing technology of sorbierite, specially a kind of new process producing high pure sorbitol using chromatographic separation technology, a kind of new process producing high pure sorbitol using chromatographic separation technology, include the following steps, starch is sized mixing, and is liquefied, saccharification, slagging-off, decoloration, ion-exchange, evaporation, hydrogenation, it is refined, chromatographic isolation, product mixed bed ion-exchange, 99 99.8% high pure sorbitols are obtained after product concentration, the raffinate obtained by chromatographic isolation refines by film concentration, allotment, mixed bed, obtains daily use chemicals grade sorbierite after concentration successively.

Description

A kind of new process producing high pure sorbitol using chromatographic separation technology
Technical field
The application belongs to the processing technology of sorbierite, specially a kind of to produce high pure sorbitol using chromatographic separation technology New process.
Background technology
D-sorbite has moisture absorption, water retention to have been widely used in food service industry tool, e.g., in chewing gum, candy production Middle addition can rise a little keeps food soft, improves tissue and reduces the effect of hardening dusting;For being retained in bread, cake Purpose;It is spoiled in logistics progress for that can be prevented in sweet food and food, moreover it is possible to chelated metal ions;For canned drink and Portugal In grape wine, it can prevent from drawing food muddiness because of metal ion.
The industrialized production of sorbierite generally has the methods of Starch Hydrolysis, bioconversion, glucose hydrogenation to be made, wherein Glucose hydrogenation is current most common production method, however this technique prepares crystalline glucose first, reaches higher pure Degree, through dissolving(Or after being purified using UF membrane, through evaporation), the crystalline sorbitol production for meeting and needing can be just produced after hydrogenation Product, the supplementary product onsumptions such as higher, complex technical process that there is production costs, technological process length, water power vapour are higher, low production efficiency The problems such as lower.
Invention content
To solve the above-mentioned problems, this application provides a kind of new works producing high pure sorbitol using chromatographic separation technology Skill, the application are realized by following proposal:
A kind of new process producing high pure sorbitol using chromatographic separation technology includes the following steps, starch is sized mixing, liquefaction, sugar Change, remove the gred, decolourize, ion-exchange is evaporated, and is hydrogenated, and is refined, chromatographic isolation, product mixed bed ion-exchange, and 99-99.8% high is obtained after product concentration Pure sorbitol, the raffinate obtained by chromatographic isolation pass through film concentration, allotment, mixed bed ion-exchange successively, after concentration daily use chemicals grade sorbierite.
Preferably, the starch is sized mixing is tuned into starch milk, and a concentration of 20-22Be` of starch milk by starch(Baume), temperature Degree be 38-46 DEG C, protein content be less than 0.4%, PH >=4.5, into liquefaction before adjustment starch concentration be 17-22Be`(Wave It is beautiful).
Preferably, the liquefaction process is by the process that Starch Hydrolysis is soluble dextrins or oligosaccharide, specially:It will form sediment Powder breast is allocated as pH to 5.2-5.8, and concentration is in 17-22 Be`(Baume), it is uniformly added into alpha-amylase online, enzyme concentration is 0.35-0.4L/ tons of sugar(Note:If do not use secondary injection, this enzyme concentration is 0.8-1L/ tons of sugar), it is uniformly mixed, through adding After hot systems are heated to 108 ± 2 DEG C, maintain be cooled to 97 ± 2 DEG C by 108 ± 2 DEG C through flash vessel within 40-90 seconds, into liquefaction It is reacted in reactor, and maintains reaction time 1.5-2 hour, liquefied into secondary injection, 125-135 DEG C of secondary injection temperature, 97 ± 2 DEG C are cooled to by 125-135 DEG C through flash vessel after maintaining 40-90 seconds, is uniformly added into 0.47L/ tons of alpha-amylase online Sugar maintains 45-60 minutes in secondary liquefying reactor, and reaction is finished is down to 60-62 DEG C through flash system flash distillation, detection DE value 12-15, adjustment pH value to 4.2-4.5, into saccharification system saccharification.
Preferably, the saccharification is that soluble dextrins or oligosaccharide that liquefaction generates are hydrolyzed to monosaccharide(Glucose)Mistake Journey, specially:Carbohydrase is added in above-mentioned liquefier online, and carbohydrase addition is 0.8-1L/ tons of sugar, maintains temperature 60-62 DEG C, reaction time 48-60 hour completes saccharification, and the final DX values that are saccharified are 95.5-96.5%, dextrin content≤0.2%.
Preferably, the slag removal is:The slag removal that saccharification terminates is the albumen and other miscellaneous removed in saccharified liquid The process of matter completes the removal of most of albumen and other impurity by plate-frame filtering method or vacuum drum filtration method, after removal of impurities Light transmittance >=80%, be visible by naked eyes impurity.
Preferably, the decolorization is:Feed liquid after slagging-off still contains certain organic pigment, needs through making a living Property carbon decoloring, activated carbon can be used powdery or granular active carbon, and the additive amount of powdery activated carbon is 1-3 kgs/tonne dry Object, bleaching temperature can be used 70-80 DEG C, and bleaching time 30-60 minutes, the light transmittance after decoloration answers >=99%.
Preferably, the ion-exchange process is:The saccharified liquid of decoloration is completed, conductivity is higher, and various ions are contained in inside, needs Ion exchange system desalination is wanted, preferably with continuous ion-exchange system or full chamber bed ion-exchange.The conductivity of after ion-exchange requires 20us/cm Within, between pH=4-5.5, light transmittance >=98%.
Preferably, the evaporation process is that the saccharified liquid of the dry concentration 30-35% of after ion-exchange is concentrated to dry concentration 50-52% removes hydrogenation system.
Preferably, the hydrogenation is by the process of glucose production sorbierite, specifically:Glucose, catalyst and hydrogen Strength mixes, in autoclave(It is intermittent)Or tubular reactor(Continous way)Middle carry out hydrogenation, reaction solution is through solid-liquid Separation, catalyst are returned flow and reuse, and Sorbitol solution enters refining step after separation of solid and liquid, it is desirable that the sorb after hydrogenation Alcohol content 95-96%;The pressure of autoclave is greater than 40 kilograms, the amount of dry matter ratio 3-8% of catalyst and glucose.
Preferably, sorbierite refining step mainly utilizes the nickel ion in ion-exchange system removal Sorbitol solution, using sun Cloudy ion-exchange system two-stage series connection operation, prevents nickel ion from entering chromatographic system across bed.Nickel ion content control after refined Within 1ppm, conductivity is less than 2um/cm.
Preferably, the chromatographic purification process is under 60-65 DEG C of running temperature, operating pressure 4bar, to sorb High pure sorbitol product of the hydride separating-purifying of alcohol content 95-96% to 99-99.8%.
The use device of the technique includes by the sequentially connected starch size mixing device of pipeline, liquefying plant, saccharification dress It sets, deslagging device, decoloration device, ion-exchange device, vaporising device, hydrogenation apparatus, refining plant, chromatographic separation device, product mix Bed ion-exchange device, product enrichment facility and 99-99.8% high pure sorbitol storage devices.
Preferably, the chromatographic separation device includes chromatographic separation device ontology, and the chromatographic separation device is intrinsic Top is equipped with horizontal upper orchestration, and the intrinsic lower part of chromatographic separation device is equipped with horizontal lower collector, described above to divide Separation resin is equipped between orchestration and lower collector.
Preferably, the upper distributor and lower collector are detachably cleared up, on the upper distributor and lower collector Equipped with aperture, aperture is uniformly distributed.
Preferably, the top of the chromatographic separation device ontology is equipped with inlet tube, and bottom is equipped with outlet, inlet tube difference Be connected with the pipeline of feed pump and intake pump, be equipped on the pipeline of feed pump and intake pump thermometric instrument, manometer and Regulating valve.
Preferably, the outlet of the chromatographic separation device ontology is equipped with the first branch pipe, the chromatographic separation device sheet Body inlet tube is equipped with the second branch pipe, and the of first branch pipe of chromatographic separation device ontology and adjacent chromatographic separation device ontology Two branch pipes are connected by connecting tube, and the connecting tube is equipped with circulating pump, and pump discharge is equipped with stop valve between ontology and different groups Divide outlet valve.
Preferably, manometer, entire chromatography are equipped on the inlet tube and outlet of the chromatographic separation device ontology Thermometric instrument and a flow instrument and a concentration instrument, chromatographic isolation there are one being set on pipeline between separator ontology Each discharge header pipe road of device is equipped with flow instrument, concentration instrument and regulating valve;
Preferably, the chromatographic separation device is connected by pipeline with raffinate storage device, and the raffinate storage device passes through Pipeline is connected with film condensing device, and the film condensing device is connected by pipeline with deployment device, and the deployment device is logical It crosses pipeline with mixed bed refining plant to be connected, the mixed bed refining plant is connected by pipeline with enrichment facility, the concentration Device is connected by pipeline with daily use chemicals sorbierite storage device.
Percentage sign in the application, which such as has no special requirements, refers both to mass percent.
The shortcomings that traditional handicraft:
1, the raw material before traditional handicraft hydrogenation is that the high-purity glucose syrup of 99.5% or more glucose content removes hydrogenation system, hydrogen The purity that sorbierite product is obtained after change can only achieve 98-99%, and raw material is glucose content before the hydrogenation of the application technique 96.5% saccharified liquid, not purified directly to remove hydrogenation system, the purity through chromatographic purification sorbierite product after hydrogenation is reachable To 99.5% or more;
2, the crystal glucose raw material that old technique uses is that complicated process generates, and process route is long, process complexity, not only at The microbiological contamination probability of this height, glucose workshop section is also high;
3, the high-purity glucose of DX99.5 is used before old technique hydrogenation, because hydrogenation system is the reaction process under high temperature, condition of high voltage, By-product is higher, so the sorbitol content after hydrogenation is only between 98.5-99%, there are about the generations of 1% by-product, influence production The purity of product;
4, old technique into before hydrogenation system, crystal glucose will pass through plus water be allocated as the Glucose Liquid of dry concentration 50-52% into The water of hydrogenation system, addition finally needs consumption steam that water is steamed out again, since accounting is very high in cost for steam, before hydrogenation Cost using high purity product is higher.
The advantages of the application technique:
1, processing line is short out:The saccharification of glucose content 96.5% is obtained only with common liquefaction, saccharification, refined, concentration means Liquid is no longer pass through the purification process such as concentration, crystallization, separation, and simple for process, input cost is low;
2, product quality is high:The present invention uses DX96.5 saccharified liquids to go hydrogenation system response for raw material before hydrogenation, although by Reacted under high-temperature and high-pressure conditions, the final sorbitol content that discharges only reaches 95-96%, but using chromatographic separation technology to impurity compared with High sorb raw polyol can obtain the high pure sorbitol product that sorbierite purity is 99.5% or more after carrying out purification & isolation;
3, operating cost is low:High pure sorbitol new process is produced using chromatographic separation technology, although adding a large amount of eluting waters, Mostly into raffinate, most of water is separated these eluting waters again after film concentrates, and can be used for used in chromatograph and washes Dehydration;Overall operation cost is lower than traditional handicraft.
4, convenient source is used before hydrogenation system(Saccharified liquid of the generally use glucose content in 96-96.5%), Gao Chunshan The acquisition of pears alcohol product is put after hydrogenation, and high pure sorbitol product, sorbierite production are obtained using chromatographic separation technology Methods For Purification The purity of product can reach 99.5% or more.Its advantage is, simple for process, and production chain is short, and operating cost is low, and product purity is high, Product quality is stablized.
Description of the drawings
Fig. 1 is the application structural schematic diagram;
Fig. 2 is chromatographic separation device structural schematic diagram;
Wherein, 1, starch size mixing device, 2, liquefying plant, 3, saccharification apparatus, 4, deslagging device, 5, decoloration device, 6, ion-exchange dress It sets, 7, vaporising device, 8, hydrogenation apparatus, 9, refining plant, 10, chromatographic separation device, 11, product mixed bed ion-exchange device, 12, production Product enrichment facility, 13,99-99.8% high pure sorbitol storage devices, 14, raffinate storage device, 15, film condensing device, 16, adjust With device, 17, mixed bed refining plant, 18, enrichment facility, 19, daily use chemicals sorbierite storage device.
Specific implementation mode
Embodiment 1
A kind of new process producing high pure sorbitol using chromatographic separation technology includes the following steps, starch is sized mixing, liquefaction, sugar Change, remove the gred, decolourize, ion-exchange is evaporated, and is hydrogenated, and is refined, chromatographic isolation, product mixed bed ion-exchange, and 99-99.8% high is obtained after product concentration Pure sorbitol, raffinate obtained by chromatographic isolation successively after film concentration, allotment, mixed bed ion-exchange, concentration daily use chemicals grade sorbierite;
Preferably, the starch is sized mixing is tuned into starch milk, and a concentration of 20-22Be` of starch milk by starch(Baume), temperature is 38-46 DEG C, protein content be less than 0.4%, PH >=4.5, into liquefaction before adjustment starch concentration be 17-22Be`(Baume);
Preferably, the liquefaction process is by the process that Starch Hydrolysis is soluble dextrins or oligosaccharide, specially:By starch milk It is allocated as pH to 5.2-5.8, concentration is in 17-22 Be`(Baume), it is uniformly added into alpha-amylase, enzyme concentration 0.35- online 0.4L/ tons of sugar(Note:If do not use secondary injection, this enzyme concentration is 0.8-1L/ tons of sugar), it is uniformly mixed, heated system After system is heated to 108 ± 2 DEG C, maintain be cooled to 97 ± 2 DEG C by 108 ± 2 DEG C through flash vessel within 40-90 seconds, into liquefaction reaction It is reacted in device, and maintains reaction time 1.5-2 hour, liquefied into secondary injection, 125-135 DEG C of secondary injection temperature maintains 97 ± 2 DEG C are cooled to by 125-135 DEG C through flash vessel after 40-90 seconds, 0.47L/ tons of sugar of alpha-amylase are uniformly added into online, two It is maintained 45-60 minutes in secondary liquefying reactor, reaction is finished is down to 60-62 DEG C through flash system flash distillation, detection DE values 12- 15, adjustment pH value to 4.2-4.5, into saccharification system saccharification;
Preferably, the saccharification is that soluble dextrins or oligosaccharide that liquefaction generates are hydrolyzed to monosaccharide(Glucose)Process, Specially:Carbohydrase is added in above-mentioned liquefier online, and carbohydrase addition is 0.8-1L/ tons of sugar, maintains 60-62 DEG C of temperature, instead Saccharification is completed within 48-60 hours between seasonable, the final DX values that are saccharified are 95.5-96.5%, dextrin content≤0.2%;
Preferably, the slag removal is:The slag removal that saccharification terminates is albumen and the other impurity removed in saccharified liquid Process completes the removal of most of albumen and other impurity by plate-frame filtering method or vacuum drum filtration method, saturating after removal of impurities Light rate >=80%, is visible by naked eyes impurity;
Preferably, the decolorization is:Feed liquid after slagging-off still contains certain organic pigment, needs by activated carbon Powdery or granular active carbon can be used in decoloration, activated carbon, and the additive amount of powdery activated carbon is 1-3 kgs/tonne of dry, is taken off Color temperature can be used 70-80 DEG C, and bleaching time 30-60 minutes, the light transmittance after decoloration answers >=99%;
Preferably, the ion-exchange process is:Complete decoloration saccharified liquid, conductivity is higher, inside contain various ions, need from Sub- exchange system desalination, preferably with continuous ion-exchange system or full chamber bed ion-exchange.The conductivity of after ion-exchange require 20us/cm with It is interior, between pH=4-5.5, light transmittance >=98%;
Preferably, the evaporation process is that the saccharified liquid of the dry concentration 30-35% of after ion-exchange is concentrated to dry concentration 50- 52% removes hydrogenation system;
Preferably, the hydrogenation is by the process of glucose production sorbierite, specifically:Glucose, catalyst and hydrogen strength Mixing, in autoclave(It is intermittent)Or tubular reactor(Continous way)Middle carry out hydrogenation, reaction solution through be separated by solid-liquid separation, Catalyst is returned flow and reuses, and Sorbitol solution enters refining step after separation of solid and liquid, it is desirable that the sorbierite after hydrogenation contains Measure 95-96%;The pressure of autoclave is greater than 40 kilograms, the amount of dry matter ratio 3-8% of catalyst and glucose;
Preferably, sorbierite refining step, mainly utilize ion-exchange system removal Sorbitol solution in nickel ion, using Yang Yin from Friendship system two-stage series connection is run, and prevents nickel ion from entering chromatographic system across bed.Nickel ion content control after refined exists Within 1ppm, conductivity is less than 2um/cm;
Preferably, the chromatographic purification process is contained to sorbierite under 60-65 DEG C of running temperature, operating pressure 4bar The hydride separating-purifying of 95-96% is measured to the high pure sorbitol product of 99-99.8%.
The sorbierite obtained after the application hydrogenation, after refined, chromatographic fractionation system can be entered by not having to concentration, purified After separation, two kinds of components are can get, one is the extracting solution parts of sorbitol content 99-99.8%, after mixed bed ion-exchange and concentration It goes other process to use as raw material, also can be used as product take-away;Isolated another component is within dry concentration 5%, Sorbitol content is in the residual liquid phase part of 55-75%, and for raffinate after film concentration systems, filtering is mutually the RO pure water after film concentration, It can directly go chromatographic system to be used as eluting water, can be used for other process;Concentration is mutually the concentration of dry concentration 9-10% The hydride of liquid and sorbitol content 95-96% after hydrogenation are deployed into the daily use chemicals grade sorbierite of various specifications, through further refining, It is taken out after concentration.
Embodiment 2
On the basis of embodiment 1, device that the technique uses include by the sequentially connected starch size mixing device 1 of pipeline, Liquefying plant 2, saccharification apparatus 3, deslagging device 4, decoloration device 5, ion-exchange device 6, vaporising device 7, hydrogenation apparatus 8, refined dress Set 9, chromatographic separation device 10, product mixed bed ion-exchange device 11, product enrichment facility 12 and the storage of 99-99.8% high pure sorbitols Device 13.
Embodiment 3
On the basis of embodiment 2, the chromatographic separation device includes chromatographic separation device ontology, the chromatographic separation device sheet Internal top is equipped with horizontal upper orchestration, and the intrinsic lower part of chromatographic separation device is equipped with horizontal lower collector, institute It states and is equipped with separation resin between distributor and lower collector.
Embodiment 4
On the basis of embodiment 3, the upper distributor and lower collector are detachably cleared up, the upper distributor and lower collection Aperture is equipped on device, aperture is uniformly distributed.
Embodiment 5
On the basis of embodiment 4, the top of the chromatographic separation device ontology is equipped with inlet tube, and bottom is equipped with outlet, enters Mouth pipe is connected with the pipeline of feed pump and intake pump respectively, and thermometric instrument, pressure are equipped on the pipeline of feed pump and intake pump Power instrument and regulating valve.
Embodiment 6
On the basis of embodiment 5, the outlet of the chromatographic separation device ontology is equipped with the first branch pipe, the chromatographic isolation Device body inlet tube is equipped with the second branch pipe, first branch pipe of chromatographic separation device ontology and adjacent chromatographic separation device sheet Second branch pipe of body is connected by connecting tube, the connecting tube be equipped with circulating pump, pump discharge be equipped with ontology between stop valve and Different component outlet valve.
Embodiment 7
On the basis of embodiment 6, it is equipped with manometer on the inlet tube and outlet of the chromatographic separation device ontology, it is whole Thermometric instrument and a flow instrument and a concentration instrument, color there are one being set on pipeline between a chromatographic separation device ontology The each discharge header pipe road for composing separator is equipped with flow instrument, concentration instrument and regulating valve.
Embodiment 8
On the basis of embodiment 7, the chromatographic separation device 10 is connected by pipeline with raffinate storage device 14, described residual Liquid storage device 14 is connected by pipeline with film condensing device 15, and the film condensing device 15 passes through pipeline and deployment device 16 It is connected, the deployment device 16 is connected by pipeline with mixed bed refining plant 17, and the mixed bed refining plant 17 passes through pipe Road is connected with enrichment facility 18, and the enrichment facility 18 is connected by pipeline with daily use chemicals sorbierite storage device 19.
The conductivity of separating-purifying to the high pure sorbitol product of 99-99.8% is less than 1um/cm, and dry concentration is according to product It is required that determining;
Residual solution after chromatographic purification, dry matter content are within 5%, and sorbitol content 55-75% needs dense by film Compression apparatus is concentrated into 9~10%, the concentrate of film concentration with refine after hydride allocated after go(Decolorization filtering, if needed It wants)Ion-exchange or mixed bed carry out(Decoloration)Desalting refinement, the daily use chemicals grade sorbierite product conductivity after refining are less than 1um/cm, light transmission Rate is more than 98%;Daily use chemicals grade sorbierite after refined is needed by evaporation concentration device, and dry matter content is promoted to 70% or more, is reached To daily use chemicals grade sorbierite standard.

Claims (10)

1. a kind of new process producing high pure sorbitol using chromatographic separation technology, which is characterized in that include the following steps, form sediment Powder is sized mixing, and is liquefied, and is saccharified, and is removed the gred, decoloration, and ion-exchange is evaporated, and is hydrogenated, and is refined, chromatographic isolation, product mixed bed ion-exchange, product concentration 99-99.8% high pure sorbitols are obtained afterwards, and the raffinate obtained by chromatographic isolation is successively after film concentration, allotment, mixed bed ion-exchange, concentration Obtain daily use chemicals grade sorbierite.
2. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The starch is sized mixing is tuned into starch milk, and a concentration of 20-22Be` of starch milk by starch(Baume), temperature is 38-46 DEG C, egg Bai Hanliang be less than 0.4%, PH >=4.5, into liquefaction before adjustment starch concentration be 17-22 Be`(Baume).
3. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The liquefaction is by the process that Starch Hydrolysis is soluble dextrins or oligosaccharide, specially:Starch milk is allocated as pH to 5.2- 5.8, concentration is in 17-22Be`(Baume), it is uniformly added into alpha-amylase online, enzyme concentration is 0.35-0.4L/ tons of sugar, and mixing is equal It is even, after heated system is heated to 108 ± 2 DEG C, maintain be cooled to 97 ± 2 DEG C by 108 ± 2 DEG C through flash vessel within 40-90 seconds, into Enter in liquefying reactor and react, and maintain reaction time 1.5-2 hour, liquefies into secondary injection, secondary injection temperature 125- 135 DEG C, 97 ± 2 DEG C are cooled to by 125-135 DEG C through flash vessel after maintaining 40-90 seconds, is uniformly added into alpha-amylase online 0.47L/ tons of sugar, maintain 45-60 minutes in secondary liquefying reactor, and reaction is finished is down to 60- through flash system flash distillation 62 DEG C, detect DE value 12-15, adjustment pH value to 4.2-4.5, into saccharification system saccharification.
4. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The saccharification is that soluble dextrins or oligosaccharide that liquefaction generates are hydrolyzed to monosaccharide(Glucose)Process, specially:It is above-mentioned Carbohydrase is added in liquefier online, and carbohydrase addition is 0.8-1L/ tons of dries, maintains 60-62 DEG C of temperature, reaction time 48- Saccharification is completed within 60 hours, the final DX values that are saccharified are 95.5-96.5%, dextrin content≤0.2%.
5. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The slagging-off is:The slag removal that saccharification terminates is the process for removing albumen and other impurity in saccharified liquid, passes through sheet frame mistake The removal of most of albumen and other impurity, light transmittance >=80% after removal of impurities, no naked eyes are completed in filter method or vacuum drum filtering Visible foreign.
6. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The decoloration is:Feed liquid after slagging-off still contains certain organic pigment, needs by activated carbon decolorizing, activated carbon can be adopted Additive amount with powdery or granular active carbon, powdery activated carbon is 1-3 kgs/tonne of dry, and 70- can be used in bleaching temperature 80 DEG C, bleaching time 30-60 minutes, the light transmittance after decoloration answers >=90%.
7. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The ion-exchange is:The saccharified liquid of decoloration is completed, conductivity is higher, and various ions are contained in inside, need ion exchange system desalination, Preferably with continuous ion-exchange system or full chamber bed ion-exchange;The conductivity of after ion-exchange requires within 20us/cm, between pH=4-5.5, Light transmittance >=98%.
8. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that It is described to be evaporated to:By the saccharified liquid of the dry concentration 30-35% of after ion-exchange, it is concentrated to dry concentration 50-52% and removes hydrogenation system;It is excellent Choosing, the hydrogenation is by the process of glucose production sorbierite, specifically:Glucose, catalyst and hydrogen strength mix, Autoclave(It is intermittent)Or tubular reactor(Continous way)Middle carry out hydrogenation, reaction solution is through being separated by solid-liquid separation, catalyst It is returned flow to reuse, Sorbitol solution enters refining step after separation of solid and liquid, it is desirable that the sorbitol content 95- after hydrogenation 96%;The pressure of autoclave is 40 kilograms or more, the amount of dry matter ratio 3-8% of catalyst and glucose;Preferably, refine is to utilize Ion-exchange system removes the nickel ion in Sorbitol solution, using positive cloudy ion-exchange system two-stage series connection operation, prevents nickel ion from passing through bed Layer enters chromatographic system;Nickel ion content after refined controls within 1ppm, and conductivity is less than 2um/cm;Preferably, described Chromatographic purification process is the hydrogenation to sorbitol content 95-96% under 60-65 DEG C of running temperature, operating pressure 4bar High pure sorbitol product of the liquid separating-purifying to 99-99.8%.
9. a kind of new process producing high pure sorbitol using chromatographic separation technology as described in claim 1, which is characterized in that The use device of the technique includes by the sequentially connected starch size mixing device of pipeline, liquefying plant, saccharification apparatus, slagging-off dress It sets, decoloration device, ion-exchange device, vaporising device, hydrogenation apparatus, refining plant, chromatographic separation device, product mixed bed ion-exchange dress It sets, product enrichment facility and 99-99.8% high pure sorbitol storage devices;
Preferably, the chromatographic separation device includes chromatographic separation device ontology, the intrinsic top of chromatographic separation device Equipped with horizontal upper orchestration, the intrinsic lower part of chromatographic separation device is equipped with horizontal lower collector, the upper distributor Separation resin is equipped between lower collector;
Preferably, the upper distributor and lower collector are detachably cleared up, and are equipped on the upper distributor and lower collector Aperture, aperture are uniformly distributed.
10. a kind of new process being produced high pure sorbitol using chromatographic separation technology as claimed in claim 9, feature are existed Be equipped with inlet tube in the top of, the chromatographic separation device ontology, bottom is equipped with outlet, inlet tube respectively with feed pump and into The pipeline of water pump is connected, and thermometric instrument, manometer and regulating valve are equipped on the pipeline of feed pump and intake pump;
Preferably, the outlet of the chromatographic separation device ontology is equipped with the first branch pipe, and the chromatographic separation device ontology enters Mouthful pipe is equipped with the second branch pipe, second of first branch pipe of chromatographic separation device ontology and adjacent chromatographic separation device ontology Pipe is connected by connecting tube, and the connecting tube is equipped with circulating pump, and pump discharge goes out equipped with stop valve between ontology and different component Expect valve;
Preferably, manometer, entire chromatographic isolation are equipped on the inlet tube and outlet of the chromatographic separation device ontology Thermometric instrument and a flow instrument and a concentration instrument, chromatographic separation device there are one being set on pipeline between device body Each discharge header pipe road be equipped with flow instrument, concentration instrument and regulating valve;
Preferably, the chromatographic separation device is connected by pipeline with raffinate storage device, and the raffinate storage device passes through Pipeline is connected with film condensing device, and the film condensing device is connected by pipeline with deployment device, and the deployment device is logical It crosses pipeline with mixed bed refining plant to be connected, the mixed bed refining plant is connected by pipeline with enrichment facility, the concentration Device is connected by pipeline with daily use chemicals sorbierite storage device.
CN201810660854.0A 2018-06-25 2018-06-25 A kind of new process producing high pure sorbitol using chromatographic separation technology Pending CN108503506A (en)

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