CN108440610A - The method for purifying deoxyribose - Google Patents
The method for purifying deoxyribose Download PDFInfo
- Publication number
- CN108440610A CN108440610A CN201810322689.8A CN201810322689A CN108440610A CN 108440610 A CN108440610 A CN 108440610A CN 201810322689 A CN201810322689 A CN 201810322689A CN 108440610 A CN108440610 A CN 108440610A
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- CN
- China
- Prior art keywords
- deoxyribose
- supercritical fluid
- extraction
- pressure
- purification
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
- C07H3/08—Deoxysugars; Unsaturated sugars; Osones
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses the techniques for purifying deoxyribose using crystalization in supercritical fluid comprising following steps：(1) 90 containing the impurity DEG C deoxyribose solution become reconciled by using raw material pump is entered from extraction extraction tower top spray, simultaneously supercritical fluid is passed through in extraction extraction tower bottom, it is 33~36 DEG C to control shooting flow temperature, and pressure is 9~11Mpa, 15~20m of flow3/min；(2) containing dissolving deoxyribose high-pressure supercritical fluid through throttle valve be depressured to less than below supercritical fluid critical pressure enter separating still；(3) after extracting deoxyribose, product is successively by dehydration, drying process.Present invention process is simple, device structure is compact, the technical process crystal is to form crystal layer in heating surface simultaneously, rather than float on a liquid, this avoid the blockings of equipment and pipeline, reduce the generation of fault in production, the product purity gone out using the technique productions is high, outer tube is bright and white, and bioactivity is good, epigranular.
Description
Technical field
The present invention relates to the methods that the method for purification of deoxyribose more particularly to supercritical fluid purify deoxyribose.
Background technology
Deoxyribose is food preservative, antistaling agent.The product to the saccharomycete in food, spoilage organisms, mould have compared with
Strong bacteriostasis is widely used in the anti-corrosion, fresh-keeping of meat, fish, greengrocery, fruits, beverage class, cake class etc., is
New-type wide-spectrum bacteriostatic agent.The equipment of the deoxyribose of large-scale production both at home and abroad is general enamel reaction still at present, ripe work
The process of skill approximately as：Take dehydroactic acid and sodium hydroxide to occur neutralization reaction, then through enamel still crystallisation by cooling, dehydration,
The processes such as dry, packaging obtain finished product, however due to the bad control of the jacketed cooling temperature of enamel still, it is easy to make material stickness, at
Product rate is not high, and purity is also affected significantly, and appearance is very secondary.Chinese patent CN102219770 is disclosed to be purified with membrane filter method
Method, but use the method, product purity still do not reach requirement.Therefore carrying for high-purity requirement can be reached by needing to provide
Pure method.
Invention content
The technical problem to be solved in the present invention is to provide the methods that supercritical fluid purifies deoxyribose, have good flat
Row reaction selectivity and safety, reduce cost and equipment investment；It is environmentally friendly, less energy consumption, and deoxyribose product is pure
Degree height, stay in grade.
In order to solve the above technical problems, the technical solution adopted by the present invention is：Supercritical fluid purifies the side of deoxyribose
Method, main includes extraction, separation, dehydration, drying process, and innovative point is：Include the following steps：
(1) 90 containing the impurity DEG C deoxyribose solution become reconciled by using raw material pump is entered from extraction extraction tower top spray,
Simultaneously supercritical fluid is passed through in extraction extraction tower bottom, control shooting flow temperature is 33~36 DEG C, pressure is 9~
11Mpa, 15~20m of flow3/ min so that deoxyribose is dissolved in supercritical fluid；
(2) high-pressure supercritical fluid of the deoxyribose containing dissolving is depressured to through throttle valve less than supercritical fluid critical pressure
Enter separating still below；
(3) after extracting deoxyribose, product by dehydration, drying process, obtains deoxyribose powder successively.
The supercritical fluid of the present invention can be carbon dioxide (CO2), CO2It is easy to get, it is cheap.
Further, the step (1) is specially：90 containing the impurity DEG C deoxyribose become reconciled by is pumped using raw material
Solution enters from extraction extraction tower top spray, while being passed through supercritical fluid in extraction extraction tower bottom, controls shooting flow temperature
It it is 33~36 DEG C, pressure is 9~11Mpa, 15~20m of flow3/ min so that deoxyribose is dissolved in supercritical fluid；
Further, the step (2) is specially：The high-pressure supercritical fluid of the deoxyribose containing dissolving is depressured through throttle valve
Enter separating still to below less than supercritical fluid critical pressure；Supercritical fluid solubility, which drastically declines, is precipitated solute, separation
At deoxyribose solution and supercritical fluid gas two parts, the former is process product, is periodically released from separating still bottom, the latter
For recyclegas, liquid recycle is condensed into through over-heat-exchanger.
Further, in the dehydration procedure of the step (3), using automatic centrifuge, it is dehydrated 30~50min, is unloaded automatically
Material；In drying process, control drying temperature is 80~90 DEG C, and drying time moisture of powder after 2.5~3.5h, drying is
8.5~10.0wt%.
Further, further include clean packaging process after the step (3).
The present invention purifies deoxyribose using supercritical fluid, has resistance small, and solution rate is fast, strong excellent of solvability
Point can obtain high-purity deoxyribose by the control to crystallization condition, and impurity is taken away with gas.
Crystalization in supercritical fluid tower purification deoxyribose of the present invention realizes crystallization and separation process integration, and what is used is molten
Agent is less, method is simple and saves the energy；Operating parameter is easily controllable；There can be selection simultaneously using continuous current method is classified
Realize efficiently separating for many kinds of substance in ground；Mass transfer velocity is fast, and extraction efficiency is high；Low temperature crystallization retains natural ingredients activity
Composition (heat-sensitive substance) and other solvents are not introduced, has been truly realized and has been crystallized the pure natural of substance；Fluid media (medium) is recyclable
It uses；It will not cause the three wastes and any environmental pollution.It is referred to as green medium；Improve crystallization safety：For using solvent
The system for recrystallizing the insecurity such as can set off an explosion, burn passes through supercritical fluid extraction columns and controls input CO2, maintain
Security of system can be improved in the optium concentration of crystallization, low-temperature operation.
Beneficial effects of the present invention：The simple for process of deoxyribose is purified by above-mentioned crystalization in supercritical fluid, is had
Good parallel reaction selectivity and safety, low-temperature operation reduce cost and equipment investment；In production process almost without
" three wastes ", it is environmentally friendly, compared with the recrystallization for using solvent, it need not dry to remove solvent, energy consumption is only rectifying
10%~30%, and deoxyribose product purity reaches 99.8% or more, stay in grade.
Description of the drawings
Fig. 1 is that the crystalization in supercritical fluid of the present invention purifies deoxyribose process flow chart.
In figure, the impure deoxyribose solution of A, B- contains the supercritical fluid of impurity, C- supercritical fluids, D- throttlings
Valve, E- extract extraction tower, F- separating stills, H- deoxyribose solution, G- heat exchangers.
Specific implementation mode
It elaborates to technical scheme of the present invention with reference to specific embodiment.
Embodiment 1
(1) the deoxyribose solution A of 90 containing impurity DEG C become reconciled by using raw material pump is from extraction extraction tower E top sprays
Enter, while supercritical fluid CO is passed through in the bottoms extraction extraction tower E2C, control shooting flow temperature is 33 DEG C, and pressure is
9Mpa, flow 15m3/ min so that deoxyribose is dissolved in supercritical fluid CO2In C；
(2) the high-pressure supercritical fluid CO of the deoxyribose containing dissolving2B is depressured to through throttle valve D less than supercritical fluid CO2
Enter separating still F below critical pressure；Supercritical fluid CO2Solubility, which drastically declines, is precipitated solute, and it is molten to be separated into deoxyribose
Liquid H and supercritical fluid gas two parts, the former is process product, is periodically released from the bottoms separating still F, the latter is circulating air
Body is condensed into liquid recycle through over-heat-exchanger G；
(3) after crystallization and purification, using automatic centrifuge, 15min, automatic discharging are dehydrated；It is 80 to control drying temperature
DEG C, i.e. acquisition deoxyribose powder is dried in 2.5h in drying time, and the moisture of powder is 9.7wt% after drying, is obtained
The purity of deoxyribose is 99.78%.
Embodiment 2
(1) the deoxyribose solution A of 90 containing impurity DEG C become reconciled by using raw material pump is from extraction extraction tower E top sprays
Enter, while supercritical fluid CO is passed through in the bottoms extraction extraction tower E2C, control shooting flow temperature is 34 DEG C, and pressure is
10Mpa, flow 17m3/ min so that deoxyribose is dissolved in supercritical fluid CO2In C；
(2) the high-pressure supercritical fluid CO of the deoxyribose containing dissolving2B is depressured to through throttle valve D less than supercritical fluid CO2
Enter separating still F below critical pressure；Supercritical fluid CO2Solubility, which drastically declines, is precipitated solute, and it is molten to be separated into deoxyribose
Liquid H and supercritical fluid gas two parts, the former is process product, is periodically released from the bottoms separating still F, the latter is circulating air
Body is condensed into liquid recycle through over-heat-exchanger G；
(3) after crystallization and purification, using automatic centrifuge, 20min, automatic discharging are dehydrated；It is 85 to control drying temperature
DEG C, i.e. acquisition deoxyribose powder is dried in 3h in drying time, and the moisture of powder is 9.2wt% after drying, and what is obtained is de-
The purity of oxygen ribose is 99.8%.
Embodiment 3
(1) the deoxyribose solution A of 90 containing impurity DEG C become reconciled by using raw material pump is from extraction extraction tower E top sprays
Enter, while supercritical fluid CO is passed through in the bottoms extraction extraction tower E2C, control shooting flow temperature is 36 DEG C, and pressure is
11Mpa, flow 20m3/ min so that deoxyribose is dissolved in supercritical fluid CO2In C；
(2) the high-pressure supercritical fluid CO of the deoxyribose containing dissolving2B is depressured to through throttle valve D less than supercritical fluid CO2
Enter separating still F below critical pressure；Supercritical fluid CO2Solubility, which drastically declines, is precipitated solute, and it is molten to be separated into deoxyribose
Liquid H and supercritical fluid gas two parts, the former is process product, is periodically released from the bottoms separating still F, the latter is circulating air
Body is condensed into liquid recycle through over-heat-exchanger G；
(3) after crystallization and purification, using automatic centrifuge, 15min, automatic discharging are dehydrated；It is 90 to control drying temperature
DEG C, i.e. acquisition deoxyribose powder is dried in 3.5h in drying time, and the moisture of powder is 8.6wt% after drying, is obtained
The purity of deoxyribose is 99.9%.
After purifying deoxyribose by using crystalization in supercritical fluid, the crystallization process of deoxyribose becomes easier to control
System, impurity is few, and the purity of finished product is higher, generally can reach 99.8% or more, and appearance is whiter and bright, and crystal is good.Pass through the technique
Improvement, there is no or greatly reduce the presence of impurity in deoxyribose finished product, effectively raise its antiseptic property, reduce
The dosage of preservative, effectively raises food security in food.
It is pointed out that the technical concepts and features of above-mentioned preferred embodiment only to illustrate the invention, its object is to
Those skilled in the art can understand the contents of the present invention and implements according to this, and the protection of the present invention can not be limited with this
Range.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.
Claims (5)
1. the method for purifying deoxyribose, main includes extraction, separation, dehydration, drying process, it is characterised in that：The method
Using supercritical fluid purifying technique, processing step is：
(1) 90 containing the impurity DEG C deoxyribose solution become reconciled by using raw material pump is entered from extraction extraction tower top spray, simultaneously
It is passed through supercritical fluid in extraction extraction tower bottom, control shooting flow temperature is 33~36 DEG C, and pressure is 9~11Mpa, stream
Measure 15~20m3/ min so that deoxyribose is dissolved in supercritical fluid；
(2) high-pressure supercritical fluid of the deoxyribose containing dissolving is depressured to through throttle valve less than below supercritical fluid critical pressure
Into separating still；
(3) after extracting deoxyribose, product by dehydration, drying process, obtains deoxyribose powder successively.
2. the method for purification deoxyribose according to claim 1, it is characterised in that：The supercritical fluid is CO2。
3. the method for purification deoxyribose according to claim 1, it is characterised in that：The step (2) is specially：Containing molten
Solve deoxyribose high-pressure supercritical fluid through throttle valve be depressured to less than below supercritical fluid critical pressure enter separating still；
Supercritical fluid solubility, which drastically declines, is precipitated solute, is separated into deoxyribose solution and supercritical fluid gas two parts, preceding
Person is process product, is periodically released from separating still bottom, the latter is recyclegas, and be condensed into liquid through over-heat-exchanger follows again
Ring.
4. the method for purification deoxyribose according to claim 1, it is characterised in that：The dehydration procedure of the step (3)
In, using automatic centrifuge, it is dehydrated 30~50min, automatic discharging；In drying process, control drying temperature is 80~90 DEG C, is done
The moisture of powder after 2.5~3.5h, drying of dry time is 8.5~10.0wt%.
5. the method for purification deoxyribose according to claim 1, it is characterised in that：Further include after the step (3)
Clean packaging process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810322689.8A CN108440610A (en) | 2018-04-11 | 2018-04-11 | The method for purifying deoxyribose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810322689.8A CN108440610A (en) | 2018-04-11 | 2018-04-11 | The method for purifying deoxyribose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108440610A true CN108440610A (en) | 2018-08-24 |
Family
ID=63199673
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810322689.8A Withdrawn CN108440610A (en) | 2018-04-11 | 2018-04-11 | The method for purifying deoxyribose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108440610A (en) |
-
2018
- 2018-04-11 CN CN201810322689.8A patent/CN108440610A/en not_active Withdrawn
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180824 |
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| WW01 | Invention patent application withdrawn after publication |