CN105153088A - Method for purifying sodium dehydroacetate - Google Patents

Method for purifying sodium dehydroacetate Download PDF

Info

Publication number
CN105153088A
CN105153088A CN201510565950.3A CN201510565950A CN105153088A CN 105153088 A CN105153088 A CN 105153088A CN 201510565950 A CN201510565950 A CN 201510565950A CN 105153088 A CN105153088 A CN 105153088A
Authority
CN
China
Prior art keywords
sodium dehydroacetate
supercritical fluid
pressure
extraction
supercutical fluid
Prior art date
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.)
Pending
Application number
CN201510565950.3A
Other languages
Chinese (zh)
Inventor
曹海涛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201510565950.3A priority Critical patent/CN105153088A/en
Publication of CN105153088A publication Critical patent/CN105153088A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
    • C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
    • C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a process for purifying sodium dehydroacetate by using supercritical fluid crystallization. The process comprises the following steps: (1) spraying neutralized impurity-containing 90 DEG C sodium dehydroacetate solution from the top of an extraction tower by using a feedstock pump, feeding supercritical fluid to the bottom portion of the extraction tower, and controlling the temperature of the supercritical fluid to be 33 to 36 DEG C, the pressure to be 9 to 11MPa and the flow to be 15 to 30m<3>/min; (2) reducing the pressure of high-pressure supercritical fluid containing dissolved sodium dehydroacetate to be below the critical pressure of the supercritical fluid through a throttling valve, and then enabling the supercritical fluid to enter a separation kettle; (3) after extraction of sodium dehydroacetate, enabling the product to sequentially pass through dehydration and drying processes. The process for purifying sodium dehydroacetate has the advantages that the process is simple and the equipment structure is compact; since the crystal layer is formed on the heat transfer surface but is not suspended in liquid during the process, the blockage of the equipment and pipes is avoided, the production faults are reduced, the purity of the product produced by using the process is high, the bioactivity is good and the grain size is uniform.

Description

The method of purification Sodium dehydroacetate
Technical field
The present invention relates to the method for purification of Sodium dehydroacetate, particularly relate to the method for supercutical fluid purification Sodium dehydroacetate.
Background technology
Sodium dehydroacetate is food preservatives, preservation agent.This product has stronger bacteriostatic action to the yeast in food, spoilage organism, mould, and being widely used in the anticorrosion, fresh-keeping of meat, fish, greengrocery, fruits, beverage class, cake class etc., is New-type wide-spectrum fungistat.The equipment of large-scale production Sodium dehydroacetate is general enamel reaction still both at home and abroad at present; the operation of its maturation process is roughly as follows: namely get dehydroacetic acid (DHA) and sodium hydroxide generation neutralization reaction; finished product is obtained again through operations such as enamel still crystallisation by cooling, dehydration, drying, packagings; but overlap the bad control of cooling temperature because enamel still adds; easily make material stickness; yield rate is not high, and purity is also affected greatly, and outward appearance is very secondary.Chinese patent CN102219770 discloses the method for purifying with membrane filter method, but adopts this method, and product purity does not still reach requirement.Therefore need to provide the method for purification that can reach high purity and require.
Summary of the invention
The technical problem to be solved in the present invention is to provide the method for supercutical fluid purification Sodium dehydroacetate, has good parallel reactor selectivity and security, reduces cost and facility investment; Environmentally friendly, less energy consumption, and Sodium dehydroacetate product purity is high, stay in grade.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the method for supercutical fluid purification Sodium dehydroacetate, mainly comprises extraction, separation, dehydration, drying process, and its innovative point is: comprise the steps:
(1) use feedstock pump by 90 DEG C of dehydroacetic acid (DHA) sodium solutions containing impurity of becoming reconciled enter from extraction extraction tower top spray, bottom extraction extraction tower, pass into supercutical fluid simultaneously, controlling supercritical flow temperature is 33 ~ 36 DEG C, and pressure is 9 ~ 11Mpa, flow 15 ~ 20m 3/ min, makes Sodium dehydroacetate be dissolved in supercutical fluid;
(2) high-pressure supercritical fluid containing dissolving Sodium dehydroacetate is depressured to through throttling valve and enters separating still lower than below supercutical fluid emergent pressure;
(3), after extraction Sodium dehydroacetate terminates, product, successively through dehydration, drying process, obtains Sodium dehydroacetate powder.
Supercutical fluid of the present invention can be carbonic acid gas (CO 2), CO 2be easy to get, low price.
Further, described step (1) is specially: use feedstock pump by 90 DEG C of dehydroacetic acid (DHA) sodium solutions containing impurity of becoming reconciled enter from extraction extraction tower top spray, bottom extraction extraction tower, pass into supercutical fluid simultaneously, controlling supercritical flow temperature is 33 ~ 36 DEG C, pressure is 9 ~ 11Mpa, flow 15 ~ 20m 3/ min, makes Sodium dehydroacetate be dissolved in supercutical fluid;
Further, described step (2) is specially: be depressured to through throttling valve containing the high-pressure supercritical fluid dissolving Sodium dehydroacetate and enter separating still lower than below supercutical fluid emergent pressure; Supercutical fluid solubleness sharply declines precipitation solute, and be separated into dehydroacetic acid (DHA) sodium solution and supercritical fluid gas two portions, the former is process product, regularly releases bottom separating still, and the latter is recycle gas, is condensed into liquid recycle through over-heat-exchanger.
Further, in the dehydration procedure of described step (3), use automatic centrifuge, dehydration 30 ~ 50min, automatic discharging; In drying process, controlling drying temperature is 80 ~ 90 DEG C, and time of drying, after dry, the moisture of powder was 8.5 ~ 10.0wt% at 2.5 ~ 3.5h.
Further, clean packaging operation is also comprised after described step (3).
The present invention utilizes supercutical fluid purification Sodium dehydroacetate, has resistance little, and dissolution rate is fast, and the advantage that dissolving power is strong, by the control to crystallization condition, can obtain high purity sodium dehydroacetate, and impurity is taken away with gas.
Crystalization in supercritical fluid tower purification Sodium dehydroacetate of the present invention achieves crystallization and sepn process integration, and the solvent of use is less, method simple and the saving energy; Operating parameters is easy to control; Utilize classification continuous flow method can realize effective separation of many kinds of substance selectively simultaneously; Mass transfer velocity is fast, and extraction efficiency is high; Low temperature crystallization, retains natural ingredients active ingredient (heat-sensitive substance), does not introduce other solvent again, really accomplished by the pure natural of crystalline material; Fluid medium can be recycled; The three wastes and any environmental pollution can not be caused.Be called as green medium; Improve crystallization security: for the system using the unsafe factors such as the recrystallization of solvent can set off an explosion, burning, by supercritical fluid extraction columns control inputs CO 2, maintain the optimum concn of crystallization, cold operation can improve security of system.
Beneficial effect of the present invention: simple by the technique of above-mentioned crystalization in supercritical fluid purification Sodium dehydroacetate, it has good parallel reactor selectivity and security, and cold operation reduces cost and facility investment; Almost do not have in production process " three wastes ", environmentally friendly, compared with using the recrystallization of solvent, do not need dry with desolvation, energy consumption is only 10% ~ 30% of rectifying, and Sodium dehydroacetate product purity reaches more than 99.8%, stay in grade.
Accompanying drawing explanation
Fig. 1 is crystalization in supercritical fluid purification Sodium dehydroacetate process flow sheet of the present invention.
In figure, the impure dehydroacetic acid (DHA) sodium solution of A, B-contains the supercutical fluid of impurity, C-supercutical fluid, D-throttling valve, and E-extracts extraction tower, F-separating still, H-dehydroacetic acid (DHA) sodium solution, G-heat exchanger.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
(1) use feedstock pump by the Sodium dehydroacetate solution A of 90 DEG C containing impurity of becoming reconciled enter from extraction extraction tower E top spray, bottom extraction extraction tower E, pass into supercutical fluid CO simultaneously 2c, controlling supercritical flow temperature is 33 DEG C, and pressure is 9Mpa, flow 15m 3/ min, makes Sodium dehydroacetate be dissolved in supercutical fluid CO 2in C;
(2) containing the high-pressure supercritical fluid CO dissolving Sodium dehydroacetate 2b is depressured to lower than supercutical fluid CO through throttling valve D 2separating still F is entered below emergent pressure; Supercutical fluid CO 2solubleness sharply declines precipitation solute, and be separated into Sodium dehydroacetate Solution H and supercritical fluid gas two portions, the former is process product, regularly releases bottom separating still F, and the latter is recycle gas, is condensed into liquid recycle through over-heat-exchanger G;
(3) after crystallization and purification terminates, automatic centrifuge is used, dehydration 15min, automatic discharging; Controlling drying temperature is 80 DEG C, carries out drying time of drying namely obtain Sodium dehydroacetate powder at 2.5h, and after dry, the moisture of powder is 9.7wt%, and the purity of the Sodium dehydroacetate obtained is 99.78%.
Embodiment 2
(1) use feedstock pump by the Sodium dehydroacetate solution A of 90 DEG C containing impurity of becoming reconciled enter from extraction extraction tower E top spray, bottom extraction extraction tower E, pass into supercutical fluid CO simultaneously 2c, controlling supercritical flow temperature is 34 DEG C, and pressure is 10Mpa, flow 17m 3/ min, makes Sodium dehydroacetate be dissolved in supercutical fluid CO 2in C;
(2) containing the high-pressure supercritical fluid CO dissolving Sodium dehydroacetate 2b is depressured to lower than supercutical fluid CO through throttling valve D 2separating still F is entered below emergent pressure; Supercutical fluid CO 2solubleness sharply declines precipitation solute, and be separated into Sodium dehydroacetate Solution H and supercritical fluid gas two portions, the former is process product, regularly releases bottom separating still F, and the latter is recycle gas, is condensed into liquid recycle through over-heat-exchanger G;
(3) after crystallization and purification terminates, automatic centrifuge is used, dehydration 20min, automatic discharging; Controlling drying temperature is 85 DEG C, carries out drying time of drying namely obtain Sodium dehydroacetate powder at 3h, and after dry, the moisture of powder is 9.2wt%, and the purity of the Sodium dehydroacetate obtained is 99.8%.
Embodiment 3
(1) use feedstock pump by the Sodium dehydroacetate solution A of 90 DEG C containing impurity of becoming reconciled enter from extraction extraction tower E top spray, bottom extraction extraction tower E, pass into supercutical fluid CO simultaneously 2c, controlling supercritical flow temperature is 36 DEG C, and pressure is 11Mpa, flow 20m 3/ min, makes Sodium dehydroacetate be dissolved in supercutical fluid CO 2in C;
(2) containing the high-pressure supercritical fluid CO dissolving Sodium dehydroacetate 2b is depressured to lower than supercutical fluid CO through throttling valve D 2separating still F is entered below emergent pressure; Supercutical fluid CO 2solubleness sharply declines precipitation solute, and be separated into Sodium dehydroacetate Solution H and supercritical fluid gas two portions, the former is process product, regularly releases bottom separating still F, and the latter is recycle gas, is condensed into liquid recycle through over-heat-exchanger G;
(3) after crystallization and purification terminates, automatic centrifuge is used, dehydration 15min, automatic discharging; Controlling drying temperature is 90 DEG C, carries out drying time of drying namely obtain Sodium dehydroacetate powder at 3.5h, and after dry, the moisture of powder is 8.6wt%, and the purity of the Sodium dehydroacetate obtained is 99.9%.
After adopting crystalization in supercritical fluid purification Sodium dehydroacetate, the crystallisation process of Sodium dehydroacetate becomes and more easily controls, and impurity is few, and the purity of finished product is higher, generally can reach more than 99.8%, and outward appearance is whiter and bright, and crystal is good.By the improvement of this technique, effectively raise its antiseptic property, reduce the consumption of sanitas in food, effectively raise food safety in Sodium dehydroacetate finished product not or greatly reduce impurity.
It is pointed out that above-mentioned preferred embodiment is only and technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.

Claims (5)

1. the method for purification Sodium dehydroacetate, mainly comprises extraction, separation, dehydration, drying process, it is characterized in that: described method adopts supercutical fluid purifying technique, and its processing step is:
(1) use feedstock pump by 90 DEG C of dehydroacetic acid (DHA) sodium solutions containing impurity of becoming reconciled enter from extraction extraction tower top spray, bottom extraction extraction tower, pass into supercutical fluid simultaneously, controlling supercritical flow temperature is 33 ~ 36 DEG C, and pressure is 9 ~ 11Mpa, flow 15 ~ 20m 3/ min, makes Sodium dehydroacetate be dissolved in supercutical fluid;
(2) high-pressure supercritical fluid containing dissolving Sodium dehydroacetate is depressured to through throttling valve and enters separating still lower than below supercutical fluid emergent pressure;
(3), after extraction Sodium dehydroacetate terminates, product, successively through dehydration, drying process, obtains Sodium dehydroacetate powder.
2. the method for purification Sodium dehydroacetate according to claim 1, is characterized in that: described supercutical fluid is CO 2.
3. the method for purification Sodium dehydroacetate according to claim 1, is characterized in that: described step (2) is specially: be depressured to through throttling valve containing the high-pressure supercritical fluid dissolving Sodium dehydroacetate and enter separating still lower than below supercutical fluid emergent pressure; Supercutical fluid solubleness sharply declines precipitation solute, and be separated into dehydroacetic acid (DHA) sodium solution and supercritical fluid gas two portions, the former is process product, regularly releases bottom separating still, and the latter is recycle gas, is condensed into liquid recycle through over-heat-exchanger.
4. the method for purification Sodium dehydroacetate according to claim 1, is characterized in that: in the dehydration procedure of described step (3), uses automatic centrifuge, dehydration 30 ~ 50min, automatic discharging; In drying process, controlling drying temperature is 80 ~ 90 DEG C, and time of drying, after dry, the moisture of powder was 8.5 ~ 10.0wt% at 2.5 ~ 3.5h.
5. the method for purification Sodium dehydroacetate according to claim 1, is characterized in that: also comprise clean packaging operation after described step (3).
CN201510565950.3A 2015-09-08 2015-09-08 Method for purifying sodium dehydroacetate Pending CN105153088A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510565950.3A CN105153088A (en) 2015-09-08 2015-09-08 Method for purifying sodium dehydroacetate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510565950.3A CN105153088A (en) 2015-09-08 2015-09-08 Method for purifying sodium dehydroacetate

Publications (1)

Publication Number Publication Date
CN105153088A true CN105153088A (en) 2015-12-16

Family

ID=54794182

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510565950.3A Pending CN105153088A (en) 2015-09-08 2015-09-08 Method for purifying sodium dehydroacetate

Country Status (1)

Country Link
CN (1) CN105153088A (en)

Similar Documents

Publication Publication Date Title
CN101781606B (en) Extraction method of rosa rugosa essential oil
CN103788041B (en) A kind of method of Sodium dehydroacetate of purifying
CN103113980A (en) Efficient extraction and purification method of mandarin peel oil
CN106752072B (en) A kind of High color values capsanthin continuous production processes
CN103694105A (en) Method for purifying sorbic acid
CN102775275A (en) Refined glycerol purification process
CN101074258B (en) Method for separating and extracting phytosterin and Vitamin E from soyabean deodorization distillate
CN204671925U (en) A kind of methanol recovery device for fluorouracil synthesis
CN111606790A (en) System and method for continuously producing high-quality and high-selectivity benzaldehyde and benzoic acid by using jet loop reactor
CN102329296B (en) Method for rectifying high-purity propylene carbonate
CN111286404A (en) Plant oil deodorizing, deacidifying and refining device and process
CN103113186B (en) Treating method and treating device for ketene dimer production residues
CN105153088A (en) Method for purifying sodium dehydroacetate
CN203998985U (en) A kind of device of producing full water-soluble sheet magnesium nitrate
CN104892389B (en) Technique for preparing oxalic acid by performing continuous reaction rectification hydrolysis on dimethyl oxalate
CN104844444A (en) Method for extracting acetic acid in salt-containing acetic acid aqueous solution by one-sided line heat integration azeotropic rectification method
CN103788127A (en) Continuous hydrolysis system for preparing glyphosate by glycine method
CN201817424U (en) Anise camphor production line
CN206486513U (en) A kind of starchy material continuous conversion equipment
CN204841334U (en) Crystal system ammonia nitrogen recovery unit
CN108440610A (en) The method for purifying deoxyribose
CN106699624A (en) Production method of lutein
CN101103805B (en) Industrial producing method for extracting fatty compound from melissa pollen
CN104356061A (en) Efficient absorption method for 2-cyanopyridine
CN105198798A (en) Production process of pyridinium hydroxy propyl sulfobetaine

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20151216

WD01 Invention patent application deemed withdrawn after publication