CN1053885C - Method for extracting mannitol from laminaria leach liquor - Google Patents
Method for extracting mannitol from laminaria leach liquor Download PDFInfo
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- CN1053885C CN1053885C CN94109352A CN94109352A CN1053885C CN 1053885 C CN1053885 C CN 1053885C CN 94109352 A CN94109352 A CN 94109352A CN 94109352 A CN94109352 A CN 94109352A CN 1053885 C CN1053885 C CN 1053885C
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Abstract
The present invention discloses a method for extracting mannitol from kelp soaking liquid under the condition of a closed cycle by combining a membrane separation combination technology and a water transportation technology. In the method, the favorable effects of reducing water consumption and energy consumption, enhancing product yield and grade quality and improving labor conditions are achieved by reasonably organizing the electrodialysis desalination technology of ion exchange membranes, the separation and impurities removal technology of ultra-filtration or micro-filtration membranes and the concentration technology of reverse osmosis membranes and the desalination technology of ion exchange resin and arranging routes of technology media (mainly water). The method is suitable for chemical industry production taking separation and extraction as contents, and has certain general significance.
Description
The present invention relates to membrane sepn chemical industry technology, specifically a kind of from marine alga, particularly kelp-soaking liquid embrane method extract the method for N.F,USP MANNITOL.
Recrystallization method extracts N.F,USP MANNITOL in the prior art from the marine alga soak solution, its crystallization concentration is more than 15%, and the content of kelp soaking water N.F,USP MANNITOL must concentrate in producing all below 2% for this reason usually, then will consume a large amount of steam or the energy in concentration process; In centrifugal water washing process repeatedly, N.F,USP MANNITOL is run off, have influence on yield.In addition, single use ion-exchange membrane electrodialysis method also can't solve the problem that energy consumption is big, yield is low.
Solve and cut down the consumption of energy, improve yield and quality problems, must resolve and purify and concentrate two problems.The present invention concentrates by the membrane sepn combination technique by strengthening processing and the purification to stoste, and the circulation of water is used in the technology, has found a reasonable approach of dealing with problems.
The objective of the invention is to provide a kind of method of from kelp-soaking liquid, extracting N.F,USP MANNITOL based on the membrane sepn combination process, it is when adopting the membrane sepn combination technique, the technical process of closed cycle is set, it has significantly and cuts down the consumption of energy, improve yield, the effect of improving the quality of products.
The method of from kelp-soaking liquid, extracting N.F,USP MANNITOL that the present invention proposes, its processing step comprises immersion, stoste is given processing, or transfers pH value and oxidation, carries iodine, desalination, the decolouring removal of impurities, concentrate and collect resultant, it is characterized in that: all technologies are condition with normal temperature, normal pressure, above-mentioned removal of impurities, concentrate, membrane separation process that desalination process consists of combination, process water is closed cycle, specifically comprises:
A, membrane sepn desalination process, wherein one-level is the ion-exchange membrane electrodialysis desalination of feed liquid, ion-exchange membrane electrodialysis and the ion exchange resin desalination associating of one-level for concentrating feed liquid;
The ultrafiltration of b, membrane separating method or micro-filtration impurity removal process;
C, reverse osmosis membrane concentration technology; And
The impure concentrated solution that d, impurity removal process discharge turns back to stoste and gives processing section and handle;
The liquid that sees through of e, reverse osmosis membrane concentration technology is guided impurity removal process, reverse osmosis membrane concentration technology itself into and is made to clean the water of water and electrodialysis desalination technology of recoiling.
Method of the present invention can be carried out separating substances and be concentrated under the condition of normal temperature, normal pressure, no phase transformation, compare with existing processes, also has following advantage:
1, saves steam, cut down the consumption of energy.Because employing combined films isolation technique has improved efficient and water liquid is fully utilized in closed cycle, saves steam, cuts down the consumption of energy.One ton of N.F,USP MANNITOL of every production can be saved 44.3 tons of steam, and amounting to expense cost is 2200 yuan.
2, improved the product yield.The product yield brings up to 10.94% from present 9.7%, has improved 12.8% N.F,USP MANNITOL yield.
3, improved quality product.Because foreign matter contents such as carbohydrate gum, organism obviously reduce in the product, the purity of product and grade improve, can be directly as medicinal.
4, alleviate labour intensity, improved production environment.
Processing method of the present invention also is applicable to separation and the extraction in other similar chemical industry, as stevioside, and the production of Xylitol.
Be described further below in conjunction with the embodiment process frame chart:
Accompanying drawing is produced the close circulation technology schematic process flow diagram of N.F,USP MANNITOL for the membrane sepn combination process.
In the block diagram shown in Figure 1,1 is soaking technology, and water soaks raw material, extract liquid, stoste after the immersion enters gives treatment process 2, remove impurity, feed liquid enters electrodialysis desalination technology 3, is at first to enter through carrying iodine usually before extracting N.F,USP MANNITOL technology again, this is in order to make full use of the useful component in the feed liquid, promptly earlier through 2.1 transferring pH value, oxidations, making iodide ion form iodine molecule, iodine are proposed through 2.2 again, surplus liquid is used for extracting N.F,USP MANNITOL.By to this feed liquid desalination, inorganic salt content in the feed liquid is dropped to≤350 mg/litre from the 15000-20000 mg/litre, (chloride content≤170 mg/litre), then enter decoloration process 4, pump into ultrafiltration then or the microfiltration membrane tripping device enters membrane separation for removing impurities technology 5, further remove impurity such as a small amount of colloid, organism, particulate, bacterium or virus remaining in the feed liquid, purify Osmitrol, for back operation reverse osmosis membrane concentrates 6 preparatory conditions, prevent to pollute.This device can use tubular type, board-like, tubular fibre formula and rolling, is best with the former interior pressure-pipe type and dismountable plate type membrane component form, the molecular weight cut-off scope 1-10 ten thousand of film, preferential 2-5 ten thousand.Feed liquid after membrane separation for removing impurities matter enters reverse osmosis membrane concentration technology 6 afterwards, concentrate and make N.F,USP MANNITOL concentrate more than 3 times, feed liquid saltiness after concentrating will increase more than 3 times, therefore utilize ion-exchange membrane electrodialysis desalination process 7 to carry out desalination again, saltiness is reduced to≤50 mg/litre, its water temperature≤30 ℃, actuating current density≤200 amperes per square meter.Remaining saltiness is removed with ion-exchange resin desalination process 8.Evaporate 9 at last, drying 10 obtains the N.F,USP MANNITOL finished product.The membrane separation for removing impurities technology of ultrafiltration or micro-filtration removal of impurities is located between ion-exchange membrane electrodialysis and the reverse osmosis membrane separation process section.
The impure water of above-mentioned technology 5 is got back to the pretreatment section removal of impurities of technology 2, despumation, water reuse; It is multiplexing that the permeate water that technology 6 is discharged is got back to fermentation vat, and small part wherein is as the recoil scavenging solution of self and the recoil scavenging solution of technology 5, and impure recoil is cleaned and handled before liquid effluent is got back to technology 2 again; Also be used as the dense water of technology 3,7, and dense water flows out discharging again as utmost point water through utmost point chamber.
Embodiment 1:
Utilize 200 * 600 millimeters of overall dimensions, 100 pairs of films are pressed the electrodialyzer of one section assembling of one-level, and a cover 4 " a rolling ultrafiltration module and a cover 4 " rolling reverse osmosis module is formed combination process by the present invention.Wherein ion-exchange membrane selects the polyethylene heterogeneous membrane, and ultra-filtration membrane selects the polysulfonamides material, and molecular weight cut-off 20,000, reverse osmosis membrane select the cellulose acetate material.
In the electrodialysis desalination water tank, put into kelp soaking water, put into the tap water of crossing through reverse-osmosis treated in dense water tank and the utmost point water tank through giving processing.Add sodium-chlor in the utmost point water, concentration 3000 mg/litre.Control electrodialysis desalination compartment flow velocity 〉=6 cels desalination that circulates.Introduce storage tank after kelp soaking water saltiness is lower than 350 mg/litre, starts ultrafiltrate pump and carry out the ultrafiltration operation, its impure concentrated solution returns the front and gives treatment process, and it is then banished through liquid and enters reverse osmosis charging liquid bath.Keep intake pressure≤0.22Mpa, discharge pressure≤0.2Mpa records 500 liters/hour of the initial flux of ultrafiltration, sees through liquid water pollution index FI≤4.0.After reverse osmosis feeding liquid case water level is raised to the appropriate location, start high-pressure pump.By heat exchanger control water temperature≤30 ℃, regulate intake pressure 2.5Mpa, top hole pressure 2.45Mpa.Record 150 liters/hour of the initial flux of permeate water, wherein mannitol content≤0.01%.Circulate after 30 minutes, record mannitol content in the concentrated solution 〉=5%.Concentrated solution through after operation to handle back gained N.F,USP MANNITOL better than the color and luster of prior art processes products obtained therefrom, the purity height.
Embodiment 2:
Adopting physical dimension is 400 * 1600 millimeters, and " the rolling counter-osmosis device is by technology component film combination process of the present invention for the thin page ultra-fine filter and 2 of the electrodialyzer that one section 200 pairs of film of one-level is assembled, 10 square metres of membrane areas of assembling.Wherein ion-exchange membrane selects the polyethylene heterogeneous membrane; Ultra-filtration membrane selects polyacrylonitrile class superpolymer, bear electricity, molecular weight cut-off 30,000; Reverse osmosis membrane selects the aromatic polyamides composite membrane.Schedule of operation is with embodiment 1.Circulate after 30 minutes, record 10 cubic metres/hour of electrodialysis water production rates, produce water saltiness≤350 mg/litre, ultrafiltration intake pressure 0.21Mpa, top hole pressure 0.20Mpa produces 1200 liters/hour of water fluxes, sees through liquid FI≤3; Reverse osmosis intake pressure 2.5Mpa, top hole pressure 2.4Mpa, the operating pressure of its suitable working range produce 25 liters/hour of water fluxes between 2.0-3.5Mpa, see through the liquid mannitol content and can not survey, and concentrated solution mannitol concentration 6% is 5 times of former kelp-soaking liquid.Concentrated solution after subsequent handling is handled compared with prior art product color brighten, purity improves.
Claims (9)
1, a kind of method of from kelp-soaking liquid, extracting N.F,USP MANNITOL, its processing step comprises immersion (1), and stoste is given processing (2), or transfers pH value and oxidation (2.1), carries iodine (2.2), desalination (3,7,8), decolouring (4), removal of impurities (5) concentrates (6) and collects resultant, it is characterized in that: all technology is condition with normal temperature, normal pressure, above-mentioned removal of impurities, concentrate, membrane separation process that desalination process consists of combination, process water is closed cycle, specifically comprises:
A, membrane sepn desalination process, wherein one-level is the ion-exchange membrane electrodialysis desalination (3) of feed liquid, ion-exchange membrane electrodialysis (7) and ion exchange resin desalination (8) associating of one-level for concentrating feed liquid;
The ultrafiltration of b, membrane separating method or micro-filtration impurity removal process (5);
C, reverse osmosis membrane concentration technology (6); And
The impure concentrated solution that d, impurity removal process discharge turns back to stoste and gives processing section and handle;
The liquid that sees through of e, reverse osmosis membrane concentration technology (6) is guided impurity removal process (5), reverse osmosis membrane concentration technology (6) itself into and is made to clean the water of water and electrodialysis desalination technology (3,7) of recoiling.
2, the method for claim 1 is characterized in that the ion-exchange membrane electrodialysis desalination process (3,7) under the normal temperature condition, its water temperature≤30 ℃, actuating current density≤200 amperes per square meter.
3, the method for claim 1 is characterized in that the membrane module form in the membrane separation for removing impurities technology (5) is a tubular type or dismountable board-like, and the molecular weight cut-off of film is 1-10 ten thousand.
4, method as claimed in claim 3, the molecular weight cut-off that it is characterized in that film is 2-5 ten thousand.
5, the method for claim 1 is characterized in that utilizing the membrane separation process (5) of ultrafiltration or micro-filtration removal of impurities to be located at butt joint up and down between ion-exchange membrane electrodialysis desalination (3) and the reverse osmosis membrane separation process section (6).
6, the method for claim 1 is characterized in that the film that uses in the reverse osmosis membrane concentration technology (6) is composite membrane.
7, as claim 1 or 6 described methods, the work operating pressure that it is characterized in that reverse osmosis membrane is 2.0-3.5Mpa.
8, the method for claim 1 is characterized in that the liquid that sees through of reverse osmosis concentration technology turns back to raw material soaking process section (1) and utilizes.
9, the method for claim 1, the dense water that it is characterized in that electrodialysis desalination technology (3,7) are drawn and are made utmost point water and use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94109352A CN1053885C (en) | 1994-08-13 | 1994-08-13 | Method for extracting mannitol from laminaria leach liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94109352A CN1053885C (en) | 1994-08-13 | 1994-08-13 | Method for extracting mannitol from laminaria leach liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1112543A CN1112543A (en) | 1995-11-29 |
| CN1053885C true CN1053885C (en) | 2000-06-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN94109352A Expired - Fee Related CN1053885C (en) | 1994-08-13 | 1994-08-13 | Method for extracting mannitol from laminaria leach liquor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402499B (en) * | 2008-10-23 | 2011-03-23 | 杭州水处理技术研究开发中心有限公司 | Method for concentrating waster solution from process for processing seafood |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811934A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of mannitol |
| CN101870639A (en) * | 2010-07-09 | 2010-10-27 | 中国水产科学研究院黄海水产研究所 | Method for producing kelp mannitol with low energy consumption |
| CN104387232A (en) * | 2014-11-11 | 2015-03-04 | 常州大学 | Method for extracting mannose from sea vegetable |
| WO2018083618A1 (en) * | 2016-11-02 | 2018-05-11 | Dahms Janine | Production of liquid biostimulants extracted from seaweed |
| CN115557828A (en) * | 2017-07-26 | 2023-01-03 | 中国水产科学研究院黄海水产研究所 | Method for treating soluble organic matters in kelp blanching water |
| CN107382666A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The efficient energy-saving extracting method of dissolved organic matter in one main laminaria blanching water |
| CN110845032A (en) * | 2019-11-01 | 2020-02-28 | 自然资源部第三海洋研究所 | Method for recycling kelp blanching liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1595832A1 (en) * | 1988-07-13 | 1990-09-30 | Московский институт народного хозяйства им.Г.В.Плеханова | Method of extracting mannite from brown algae |
-
1994
- 1994-08-13 CN CN94109352A patent/CN1053885C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1595832A1 (en) * | 1988-07-13 | 1990-09-30 | Московский институт народного хозяйства им.Г.В.Плеханова | Method of extracting mannite from brown algae |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402499B (en) * | 2008-10-23 | 2011-03-23 | 杭州水处理技术研究开发中心有限公司 | Method for concentrating waster solution from process for processing seafood |
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| CN1112543A (en) | 1995-11-29 |
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