CN107573441B - A kind of preparation method and application suitable for industrialized production high-purity sodium alginate - Google Patents
A kind of preparation method and application suitable for industrialized production high-purity sodium alginate Download PDFInfo
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 121
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 121
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 121
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000007788 liquid Substances 0.000 claims abstract description 62
- 238000000926 separation method Methods 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 43
- 235000019441 ethanol Nutrition 0.000 claims abstract description 36
- 238000005406 washing Methods 0.000 claims abstract description 29
- 238000004042 decolorization Methods 0.000 claims abstract description 21
- 238000010612 desalination reaction Methods 0.000 claims abstract description 20
- 238000005342 ion exchange Methods 0.000 claims abstract description 19
- 238000001471 micro-filtration Methods 0.000 claims abstract description 18
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 18
- 239000011575 calcium Substances 0.000 claims abstract description 16
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 16
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005352 clarification Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims description 50
- 239000000648 calcium alginate Substances 0.000 claims description 48
- 235000010410 calcium alginate Nutrition 0.000 claims description 48
- 229960002681 calcium alginate Drugs 0.000 claims description 48
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 241000512259 Ascophyllum nodosum Species 0.000 claims description 23
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 21
- 239000000706 filtrate Substances 0.000 claims description 16
- 239000004744 fabric Substances 0.000 claims description 14
- 239000012141 concentrate Substances 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000011780 sodium chloride Substances 0.000 claims description 11
- 238000004061 bleaching Methods 0.000 claims description 10
- 239000001110 calcium chloride Substances 0.000 claims description 10
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 235000010443 alginic acid Nutrition 0.000 claims description 9
- 229920000615 alginic acid Polymers 0.000 claims description 9
- 229960001126 alginic acid Drugs 0.000 claims description 7
- 239000000783 alginic acid Substances 0.000 claims description 7
- 150000004781 alginic acids Chemical class 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 241001474374 Blennius Species 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000011859 microparticle Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229920003169 water-soluble polymer Polymers 0.000 claims description 4
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 3
- 229930195725 Mannitol Natural products 0.000 claims description 3
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 3
- 239000000594 mannitol Substances 0.000 claims description 3
- 235000010355 mannitol Nutrition 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 102000004169 proteins and genes Human genes 0.000 claims description 3
- 108090000623 proteins and genes Proteins 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 150000001413 amino acids Chemical class 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000012634 fragment Substances 0.000 claims description 2
- 229920001542 oligosaccharide Polymers 0.000 claims description 2
- 150000002482 oligosaccharides Chemical class 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000001814 pectin Substances 0.000 claims description 2
- 235000010987 pectin Nutrition 0.000 claims description 2
- 229920001277 pectin Polymers 0.000 claims description 2
- 235000000346 sugar Nutrition 0.000 claims description 2
- 235000001014 amino acid Nutrition 0.000 claims 1
- 235000018102 proteins Nutrition 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 15
- 238000000746 purification Methods 0.000 abstract description 12
- 238000002955 isolation Methods 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 53
- 229960004756 ethanol Drugs 0.000 description 27
- 239000012535 impurity Substances 0.000 description 18
- 230000008569 process Effects 0.000 description 12
- 239000002253 acid Substances 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
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- 238000002203 pretreatment Methods 0.000 description 5
- 102000004190 Enzymes Human genes 0.000 description 4
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- 150000002500 ions Chemical class 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- 239000004615 ingredient Substances 0.000 description 3
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- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007071 enzymatic hydrolysis Effects 0.000 description 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 2
- 238000012869 ethanol precipitation Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000002419 base digestion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 229960000935 dehydrated alcohol Drugs 0.000 description 1
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- 239000002778 food additive Substances 0.000 description 1
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- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
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- 241000894007 species Species 0.000 description 1
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Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of preparation method and applications suitable for industrialized production high-purity sodium alginate, method includes the following steps: micro-filtration clarification, calcium are coagulated, are separated by solid-liquid separation, ethyl alcohol dissolves decoloration, washing, ion exchange, desalination and concentration by ultrafiltration, low concentration secondary decolourization and are precipitated-are separated by solid-liquid separation, dry and crush.The present invention provides the preparation method and applications of a set of high-purity fucoidin suitable for industrial-scale production.The technology of the present invention equipment sufficiently bases oneself upon sodium alginate production equipment situation, the target that purifying obtains high-purity high-quality sodium alginate product is reached by ingenious combination with conventional isolation and purification method, there is guidance and realistic meaning for the technology and product up-gradation that promote sodium alginate industry.
Description
Technical field
The present invention relates to a kind of preparation methods suitable for industrialized production high-purity sodium alginate, belong to polysaccharide purification technology
Field.
Background technique
Sodium alginate (also known as sodium alginate, algin) is a kind of hydrophilic colloid, has stabilizing cell membrane and protein
The function of structure, and with its good biological degradability and biocompatibility, be widely used in food, medicine, chemistry,
Weaving, printing and dyeing, papermaking, biology, daily-use chemical industry etc..It can be used as stabilizer, thickener, emulsifier, gelling in food
Agent, binder and functional additive use.Currently, the extraction and purification process of sodium alginate mainly takes postdigestive acid
Solidifying-acidization, calcium is solidifying-and acidization, calcium is solidifying-the new work such as traditional handicrafts and enzymatic isolation method and ultrafiltration extraction method such as ion-exchange
Skill.Sodium alginate recovery rate that Different Extraction Method obtains, purity are all different.Cost is relatively low for conventional method, but soda acid disappears
Consumption is big, high pollution, product quality be not high；New process higher cost, but low acid and alkali consumption, low pollution, product quality are higher, it can
To say each its advantage of tool.The commonly used technique of most of manufacturer is using kelp at present in China, and to be raw material through digestion-calcium coagulate-
Acidification production sodium alginate, this method calcium analyse fast speed, and precipitating particle is larger.Decalcification process need to be added a large amount of hydrochloric acid, generate compared with
More seaweed acid coagulums, and alginic acid is unstable, it is degradable, cause sodium alginate recovery rate low, product quality is low.In addition,
There is the method that high-purity sodium alginate is produced by adsorption-edulcoration using (ZL200910256451.0) such as active carbons, but so far still
Practical application is not obtained.Filtrate is decolourized after the open enzyme of Song Yanxian, Min Yutao et al. helps the residue of extraction to digest, calcium is solidifying and ion
Decalcification is exchanged, the method for purifying sodium alginate with dehydrated alcohol, but analyzed through the present inventor, when according to the big rule of the process
When mould produces sodium alginate, production efficiency is low, it is difficult to be applied in large-scale industrial production.Therefore need to develop novel fit
In the preparation method of the high-purity sodium alginate of industrialized production.
Summary of the invention
To solve the above-mentioned problems, the present invention using calcium it is solidifying-ion exchange is that core combines modern times membrane technology, according to sea
Different impurities in mosanom extracting solution isolate and purify the optimum organization of impurity-removing method by difference, develop a kind of suitable for work
The preparation method of industry metaplasia production of high purity sodium alginate.This method is suitable for various as the alkali digestion of raw material, enzyme process etc. using kelp
Sodium alginate extracts the obtained sodium alginate extracting solution of pre-processing, and extraction process does not generate any impurity, solvent for use toxicity
Low, target product alginate purity high impurity content is low, and whiteness is high, and solution transparency is high, is a kind of suitable for industrialized production
The environment-friendly type high-purity sodium alginate preparation process of application.
The technical solution adopted by the present invention is that:
The first aspect of the invention provides a kind of preparation method suitable for industrialized production high-purity sodium alginate, packet
Include following steps:
(1) kelp sodium alginate extracting solution is subjected to micro-filtration clarification, obtains clear yellowish-brown sodium alginate extracting solution；
The clear condition of micro-filtration is: the aperture of ceramic micro filter film is 50~500nm, material liquid pH 8.0~9.0, feed liquid temperature
35~45 DEG C, 0.15~0.4MPa of operating pressure, the water washing and micro-filtration of gained trapped fluid 2~3 times of volumes of filtrate；
(2) CaCl of 15~20% (w/v) is added into above-mentioned clear yellowish-brown sodium alginate extracting solution2Solution,
CaCl2Addition quality be kelp material quality used 15~25% (w/w), being stirred continuously makes calcium alginate Precipitation,
CaCl is added230~60min is stood after solution to be made to precipitate aging；
(3) filtering calcium alginate suspension obtains calcium alginate solid；
(4) it is solid that light yellow calcium alginate is obtained using high concentration ethanol washing decoloration to the calcium alginate after separation of solid and liquid
Body；
(5) the light yellow calcium alginate through high concentration ethanol washing decoloration is utilized into pure water washing；
(6) sodium alginate is converted for gained calcium alginate using ion-exchange, separation of solid and liquid obtains high saliferous seaweed
Sour sodium solid；
(7) obtained high saliferous sodium alginate solid is dissolved in pure water, desalination and concentration by ultrafiltration obtains yellowish sea
Mosanom concentrate solution；
(8) ethyl alcohol to setting concentration is added into obtained yellowish sodium alginate concentrate solution further to decolourize and precipitate
Sodium alginate washs sodium alginate using the ethanol solution of same concentrations after separation of solid and liquid, obtains high-purity sodium alginate solid；
(9) dry to obtained above-mentioned sodium alginate and crush, obtain the sodium alginate product of high-purity.
The second aspect of the invention also provides a kind of high-purity sodium alginate production being prepared using the above method
Product.
The third aspect of the invention, also the offer above method answering in industrialized production high-purity sodium alginate product
With.
Compared with prior art, technical solution of the present invention has the following beneficial effects:
(1) it the present invention provides the preparation method of a set of high-purity fucoidin suitable for industrial-scale production and its answers
With.The technology of the present invention equipment sufficiently bases oneself upon sodium alginate production equipment situation, passes through ingenious combination with conventional isolation and purification method
The target for reaching production high-purity high-quality sodium alginate product, for promoting sodium alginate level of industrial technology and product up-gradation
With directive significance.
(2) advantage outstanding of the technology of the present invention is the selection and combination by isolation technics, substantially reduces separation
The addition type and additive amount of other substances, are especially reduction of the yield of the waste liquids such as acid, alkali, with high salt in purification process,
Realize sodium alginate efficient green chemical industry production.
(3) high-purity sodium alginate technology of preparing of the present invention increases microfiltration of ceramic membrane and ultrafiltration two compared with the prior art
A link substantially increases the controllable continuous of overall technology technique, significantly improves the quality of sodium alginate.
(4) linking of the technology of the present invention link flexibly, can produce the sodium alginate product of different size, according to product market need
It asks, technical grade, food-grade and medicine can be produced on same production line by the various combination and control of sport technique segment
The different sodium alginate products such as grade, do not need other supplementary technology links.
(5) the technology of the present invention method mild condition is suitable for carrying out coproduction with other kelp functional ingredients, such as high additional
Fucoidin, mannitol, kelp dietary fiber and other microelements of value etc. realize the high-efficiency comprehensive utilization of kelp resource.
Detailed description of the invention
It constitutes a part of Figure of description of the invention to be used to provide further understanding of the present invention, signal of the invention
Examples and descriptions thereof are used to explain the present invention for property, does not constitute improper limitations of the present invention.
Fig. 1 is process flow chart of the invention.
Specific embodiment
It is noted that described further below be all exemplary, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation and/or their combination.
As background technique is introduced, there are recovery rates for the process of extraction purification sodium alginate in the prior art
Low, the disadvantages of purity is lower, therefore these existing technical methods are not appropriate for the large-scale industrial production of sodium alginate, are
Solution above-mentioned technical problem, the invention proposes a kind of preparation method suitable for industrialized production high-purity sodium alginate.
The present inventor analyzes the process of extraction purification sodium alginate in the prior art, analyzes these methods and deposits
The reason of the disadvantage mentioned above, after discovery is using pre-treatments such as conventional digestion, acid cure, enzymatic hydrolysis, then be separated by solid-liquid separation and remove sea
With the sodium alginate extracting solution obtained after slag, appearance is the thick opaque liquid of dark brown, has very more dopant species.
Contain a large amount of water insoluble microparticles (cell fragment, undissolved alginic acid, flocculation albumen, insoluble pigment through inventor's analysis
Deng), water soluble polymer (fucoidin, pectin, water-solubility protein, water colo(u)r etc.), soluble small molecular (oligosaccharides, list
Sugar, mannitol, amino acid etc.) and water-soluble inorganic salt.And process in the prior art there is no to its one by one into
Row removal, causes the quality of sodium alginate product lower.
The present inventor is exactly according to the impurity compositing characteristic in sodium alginate extracting solution, from being capable of extensive industrial application
Angle on, select and optimize separating and purifying technology and equipment, concrete technology technology is as follows:
(1) micro-filtration is clarified: kelp raw material (including complex enzyme hydrolysis-solid-liquid point after the pre-treatments such as digestion, acid cure, enzymatic hydrolysis
From method, pre-treatment-digestion-solid-liquid isolation method or pre-treatment-ultrasonic wave added digestion-solid-liquid isolation method), then be separated by solid-liquid separation and remove
The sodium alginate extracting solution for needing to be further purified is obtained after going kelp residue, appearance is the thick opaque liquid of dark brown, warp
Analysis contains a large amount of water insoluble microparticles, water soluble polymer, soluble small molecular and water-soluble inorganic salt.According to impurity
Feature, in order to later separation purifying efficient progress, the present invention selection first use micro-filtration film process sodium alginate extracting solution,
To achieve the purpose that remove water insoluble microparticle clarification extracting solution and partial decolorization.
Preferably, the clear condition of sodium alginate extracting solution micro-filtration is: the aperture of ceramic micro filter film be 50~
500nm, material liquid pH 8.0~9.0,35~45 DEG C of feed liquid temperature, 0.15~0.4MPa of operating pressure, gained trapped fluid is with filtrate 2
The water washing and micro-filtration of~3 times of volumes.
Merge all filtrates and obtain the clear sodium alginate extracting solution of yellowish-brown, carries out later separation purification process.
(2) calcium is solidifying
After obtaining clear sodium alginate extracting solution, it can be removed by precipitating alginic acid or one step of calcium alginate soluble miscellaneous
Matter can also be realized by ethanol precipitation.But confirm that precipitating alginic acid reduces the yield of final sodium alginate by practice, it is miscellaneous
Matter content is high, while destroying kelp functional ingredient fucoidin, significantly reduces it and extracts yield, is unfavorable for kelp resource high-efficiency
Comprehensive utilization；The purity of target product sodium alginate will be significantly affected by directly carrying out ethanol precipitation, be retained wherein a large amount of
Impurity, based on the above reasons, the present invention is preferred plus the isolation and purification method of calcium precipitate calcium alginate, to remove most water
Solubility impurity.
Preferably, the solidifying concrete operations of the calcium are: it is added 15 in the clear sodium alginate extracting solution of yellowish-brown~
The CaCl of 20% (w/v)2Solution, CaCl2Addition quality be kelp material quality used 15~25% (w/w), be stirred continuously
Make calcium alginate Precipitation, speed of agitator is 150~300r/min, has added CaCl2Standing 30~60min afterwards keeps precipitating old
Change, into subsequent separation of solid and liquid, removes soluble impurity.
(3) it is separated by solid-liquid separation
The convenience of current industrial production operation is combined according to the characteristic of calcium alginate precipitating, the present invention selects at filtering
Reason completes the separation of solid and liquid of calcium alginate suspension.
Preferably, the operating condition of the filtering is: filter cloth aperture is 200~400 mesh, and gained filter cake is added 2~3 times
Water washing 2~3 times, gained greenish yellow solid filter cake is calcium alginate, and resulting whole filtrate is additional for kelp height after mixing
Value functional components fucoidin and microelement isolate and purify.
(4) ethanol decolorization
By calcium it is solidifying-be separated by solid-liquid separation after eliminate water-solubility impurity, but to be that yellow green still contains more for gained calcium alginate
Pigment impurity, it is therefore desirable to it decolourizes, the active carbon adsorption of common discoloration method, oxidation-reduction method, solvent dissolution method
Deng, because calcium alginate is solid, it is not suitable for activated carbon adsorption, and oxidation-reduction method will introduce or generate other impurities, therefore
The present invention selects to carry out calcium alginate decoloration with the ethanol washing method that food industry is common and is easily isolated.
Preferably, the condition of the ethanol decolorization is: final concentration of 65~85% (v/v) of high concentration ethanol, decoloration temperature
Degree is 35~50 DEG C, and bleaching time is 30~90min, decolorization 1~3 time, obtains light yellow calcium alginate solid.
(5) it washs
The light yellow calcium alginate to decolourize through high concentration ethanol is washed with water 1~3 time, removes water-solubility impurity.
(6) ion exchange
Sodium alginate is converted for gained calcium alginate using ion-exchange, processing step is simple, avoids a large amount of soda acids
Use.
Preferably, the condition of the ion exchange is: the additive amount of calcium alginate is 5~10% (w/v), and NaCl concentration is
15~20% (w/v), pH are 6.0~7.5, and switching architecture temperature is 35~55 DEG C, 20~60min of swap time, speed of agitator
100~300r/min, calcium alginate are changed into sodium alginate by ion exchange, and sodium alginate is in high concentration salt solutions with solid
Body precipitation form exists, and calcium ion then enters in solution, is separated by solid-liquid separation to obtain high saliferous sodium alginate solid by plate-frame filtering, adopts
With the NaCl solution of same concentrations wash gained it is saliferous sodium alginate solid 2-3 times high so that ion exchange is complete, and remove calcium
Ion.
Preferably, it is 300~500 mesh that the condition of above-mentioned plate-frame filtering, which is filter cloth aperture,.
(7) desalination and concentration by ultrafiltration
Contain a large amount of NaCl through the resulting sodium alginate solid of ion exchange, it is therefore desirable to carry out de-salting operation.In order to
It reduces operating procedure and reduces post precipitation solvent usage, the present invention selects to dissolve using by the high saliferous sodium alginate solid of gained
Desalination is carried out by ultrafiltration afterwards to be concentrated simultaneously.
To reach better desalination and concentration effect, it is preferred that the actual conditions of the desalination and concentration by ultrafiltration: high saliferous seaweed
The concentration of ordinary dissolution of sour sodium solid is 0.2~0.8% (w/v), and ultrafiltration retaining molecular weight is 1000~5000Da, temperature of charge 30
~38 DEG C, 0.15~0.5MPa of operating pressure, extracting solution cycles of concentration is 5~10 times, and gained concentrate uses 3~5 times of volumes
Water washing 2~3 times, so that desalination is complete.
(8) it low concentration secondary decolourization and precipitates-is separated by solid-liquid separation
It is further decolourized in the sodium alginate concentrate addition ethyl alcohol obtained through desalination and concentration by ultrafiltration to a certain concentration
And sodium alginate is precipitated, it is washed sodium alginate soln 1~3 time, is obtained white using the ethanol solution of same concentrations after separation of solid and liquid
Sodium alginate solid material, into drying section.
To realize better decolorizing effect, it is preferred that final concentration of 20~35% (v/v) of the addition ethyl alcohol, precipitating
Bleaching time is 30~120min, and system temperature is 25~35 DEG C；
Preferably, described be separated by solid-liquid separation uses flame filter press, and the aperture of filter cloth is 300~500 mesh.
(9) it dries and crushes
Preferably, drying condition is 70~90 DEG C, and drying time is 2~4h.
Through above-mentioned method for preparing purified, gained sodium alginate product is off-white color to white, and whiteness > 85% is average to recycle
Rate >=98%, water-insoluble < 0.3%, purity 98-99.5%.The present invention is by there is isolation technics in the prior art
Imitate selection and combination, improve sodium alginate quality on and reduce waste liquid in terms of achieve unexpectedly
Technical effect, realize the efficiently purifying of sodium alginate.
In order to enable those skilled in the art can clearly understand technical solution of the present invention, below with reference to tool
The embodiment and the comparative example technical solution that the present invention will be described in detail of body.
Embodiment 1
After impregnating pre-treatment by washing, the sodium alginate extracting solution obtained through complex enzyme hydrolysis-separation of solid and liquid, technique
Process is as shown in Figure 1:
(1) micro-filtration clarify: the aperture of ceramic micro filter film be 100nm, material liquid pH 8.5,35 DEG C of feed liquid temperature, operating pressure
0.4MPa, gained trapped fluid are washed and micro-filtration with the deionized water of 3 times of volumes of filtrate, and merging all filtrates, to obtain yellowish-brown clear
Sodium alginate extracting solution carries out later separation purification process.
(2) calcium is solidifying: the CaCl of 20% (w/v) being added in the clear sodium alginate extracting solution of yellowish-brown2Solution, CaCl2's
25% (w/w) that quality is kelp material quality used is added, being stirred continuously makes calcium alginate Precipitation, speed of agitator
200r/min has added CaCl2Standing 60min afterwards makes to precipitate aging, and into subsequent separation of solid and liquid, it is soluble to remove the overwhelming majority
Impurity.
(3) be separated by solid-liquid separation: the operating condition of plate-frame filtering be filter cloth aperture be 400 mesh, gained filter cake be added 3 times go from
Sub- water washing 2 times, gained greenish yellow solid filter cake are calcium alginate, and resulting whole filtrate is used for kelp high added value after mixing
Functional components fucoidin and microelement etc. isolate and purify.
(4) ethanol decolorization: final concentration of 85% (v/v) of high concentration ethanol, bleaching temperature are 50 DEG C, and bleaching time is
90min decolorization 3 times, obtains light yellow calcium alginate solid.
(5) wash: the light yellow calcium alginate solid to decolourize through high concentration ethanol is washed with deionized 3 times, removes water
Solubility impurity.
(6) ion exchange-separation of solid and liquid: the additive amount of calcium alginate is 5% (w/v), and NaCl concentration is 16% (w/v),
PH is 6.5, and switching architecture temperature is 45 DEG C, swap time 60min, speed of agitator 250r/min, and calcium alginate is handed over by ion
It changes and is changed into sodium alginate；It is separated by solid-liquid separation and uses flame filter press, the aperture of filter cloth is 400 mesh, and gained filter cake is using identical dense
The NaCl solution deep ion exchange of degree washing 3 times, obtains high saliferous sodium alginate solid material.
(7) desalination and concentration by ultrafiltration: the high dissolved concentration of saliferous sodium alginate solid is 0.2% (w/v), ultrafiltration membrane retention
Molecular weight is 1000Da, and 38 DEG C of temperature of charge, operating pressure 0.25MPa, extracting solution cycles of concentration is 5 times, and gained concentrate is with 5
The deionized water of times volume is washed 3 times, so that desalination is complete.Yellowish sodium alginate concentrate solution is obtained after concentrated desalination.
(8) it low concentration secondary decolourization and precipitates-is separated by solid-liquid separation: adding final concentration of 35% (v/v) of ethyl alcohol, precipitate and decolorization
When 120min, system temperature be 35 DEG C；It is separated by solid-liquid separation and uses flame filter press, the aperture of filter cloth is 300 mesh；It is adopted after separation of solid and liquid
It is washed sodium alginate soln 3 times with the ethanol solution of same concentrations, white sodium alginate solid material is obtained, into drying section.
(9) dry and crush: drying condition is 80 DEG C of dry 4h.
Through above-mentioned method for preparing purified, gained sodium alginate is white, and whiteness reaches 95%, and the rate of recovery 99.5%, water is not
Molten object 0.1%, purity 99.3%, product quality reach the requirement of pharmaceutical grade sodium alginate.
Embodiment 2
After impregnating pre-treatment by washing, the sodium alginate extracting solution that digestion-separation of solid and liquid obtains, process flow is such as
Shown in Fig. 1:
(1) micro-filtration clarify: the aperture of ceramic micro filter film be 200nm, material liquid pH 9.0,45 DEG C of feed liquid temperature, operating pressure
0.20MPa, gained trapped fluid drink water washing and micro-filtration with 2 times of volumes of filtrate, merge all filtrates and obtain yellowish-brown clarification
Sodium alginate extracting solution, carry out later separation purification process.
(2) calcium is solidifying: the CaCl of 18% (w/v) being added in the clear sodium alginate extracting solution of yellowish-brown2Solution, CaCl2's
20% (w/w) that quality is kelp material quality used is added, being stirred continuously makes calcium alginate Precipitation, speed of agitator
250r/min has added CaCl2Standing 40min afterwards makes to precipitate aging, and into subsequent separation of solid and liquid, it is soluble to remove the overwhelming majority
Impurity.
(3) be separated by solid-liquid separation: the operating condition of plate-frame filtering is that filter cloth aperture is 300 mesh, and 2 times of gained filter cake addition is drunk
Water water washing 3 times, gained greenish yellow solid filter cake is calcium alginate, and resulting whole filtrate is used for kelp high added value after mixing
Functional components fucoidin and microelement isolate and purify.
(4) ethanol decolorization: final concentration of 75% (v/v) of high concentration ethanol, bleaching temperature are 40 DEG C, and bleaching time is
60min decolorization 2 times, obtains light yellow calcium alginate solid.
(5) wash: the light yellow calcium alginate solid through high concentration ethanol decoloration is removed water-soluble with drinking water washing 3 times
Property impurity.
(6) ion exchange: the additive amount of calcium alginate is 8% (w/v), and NaCl concentration is 18% (w/v), pH 7.0, is handed over
Changing system temperature is 40 DEG C, swap time 40min, speed of agitator 200r/min, and calcium alginate is changed into sea by ion exchange
Mosanom；It is separated by solid-liquid separation and uses flame filter press, the aperture of filter cloth is 300 mesh, and gained filter cake is molten using the NaCl of same concentrations
The exchange of liquid deep ion washing 3 times, obtain high saliferous sodium alginate solid material.
(7) desalination and concentration by ultrafiltration: the high dissolved concentration of saliferous sodium alginate solid is 0.5% (w/v), ultrafiltration membrane retention
Molecular weight is 3000Da, and 35 DEG C of temperature of charge, operating pressure 0.22MPa, extracting solution cycles of concentration is 8 times, and gained concentrate is with 3
Times volume is drunk water washing 2 times, so that desalination is complete.Yellowish sodium alginate concentrate solution is obtained after concentrated desalination.
(8) it low concentration secondary decolourization and precipitates-is separated by solid-liquid separation: adding final concentration of 25% (v/v) of ethyl alcohol, precipitate and decolorization
Time is 60min, and system temperature is 30 DEG C；It is separated by solid-liquid separation and uses flame filter press, the aperture of filter cloth is 300~500 mesh；Solid-liquid
It is washed sodium alginate soln 3 times after separation using the ethanol solution of same concentrations, white sodium alginate solid material is obtained, into drying
Workshop section.
(9) it dries and crushes
Preferably, drying condition is 90 DEG C, drying time 3h.
Through above-mentioned method for preparing purified, gained sodium alginate is white, whiteness 92%, the rate of recovery >=99.2%, and water is insoluble
Object 0.22%, purity 98.5%, product quality indicator meet national food safety standard food additives sodium alginate (also known as
Sodium alginate) GB1886.243-2016 regulation.
Embodiment 3
After through pre-treatments such as washing immersions, the sodium alginate extracting solution that ultrasonic wave added digestion-separation of solid and liquid obtains,
Process flow is as shown in Figure 1:
(1) micro-filtration clarify: the aperture of ceramic micro filter film be 300nm, material liquid pH 9.0,45 DEG C of feed liquid temperature, operating pressure
0.15MPa, the originally water washing of gained trapped fluid 2 times of volumes of filtrate and micro-filtration, merging all filtrates, to obtain yellowish-brown clear
Sodium alginate extracting solution carries out later separation purification process.
(2) calcium is solidifying: the CaCl of 15% (w/v) being added in the clear sodium alginate extracting solution of yellowish-brown2Solution, CaCl2's
15% (w/w) that quality is kelp material quality used is added, being stirred continuously makes calcium alginate Precipitation, speed of agitator
300r/min has added CaCl2Standing 30 afterwards makes to precipitate aging, into subsequent separation of solid and liquid, removes soluble impurity.
(3) be separated by solid-liquid separation: the operating condition of plate-frame filtering is that filter cloth aperture is 200 mesh, and gained filter cake is added 2 times originally
Water washing 2 times, gained greenish yellow solid filter cake is calcium alginate, and resulting whole filtrate is used for kelp high added value function after mixing
Can property ingredient fucoidin and microelement isolate and purify.
(4) ethanol decolorization: final concentration of 65% (v/v) of high concentration ethanol, bleaching temperature are 35 DEG C, and bleaching time is
30min decolorization 2 times, obtains yellow calcium alginate solid.
(5) wash: light yellow calcium alginate solid originally water washing 2 times decolourized through high concentration ethanol remove water-soluble
Property impurity.
(6) ion exchange: the additive amount of calcium alginate be 10% (w/v), NaCl concentration be 20% (w/v), pH 7.5,
Switching architecture temperature is 50 DEG C, swap time 35min, speed of agitator 300r/min, and calcium alginate is changed by ion exchange
Sodium alginate；It is separated by solid-liquid separation and uses flame filter press, the aperture of filter cloth is 300 mesh, and gained filter cake uses the NaCl of same concentrations
Solution deep ion-exchange detergency 2 times, obtain high saliferous sodium alginate solid material.
(7) desalination and concentration by ultrafiltration: the high dissolved concentration of saliferous sodium alginate solid is 0.8% (w/v), ultrafiltration membrane retention
Molecular weight is 5000Da, and 35 DEG C of temperature of charge, operating pressure 0.15MPa, extracting solution cycles of concentration is 5 times, and gained concentrate is with 3
Originally water washing 1 time of times volume, so that desalination is complete.Yellowish sodium alginate concentrate solution is obtained after concentrated desalination.
(8) it low concentration secondary decolourization and precipitates-is separated by solid-liquid separation: adding final concentration of 22% (v/v) of ethyl alcohol, precipitate and decolorization
Time is 45min, and system temperature is 35 DEG C；It is separated by solid-liquid separation and uses flame filter press, the aperture of filter cloth is 300 mesh；It is separated by solid-liquid separation
It is washed sodium alginate soln 1 time using the ethanol solution of same concentrations afterwards, white sodium alginate solid material is obtained, into back tender
Section.
(9) dry and crush: drying condition is 90 DEG C of dry 2h.
Through above-mentioned method for preparing purified, gained sodium alginate is off-white color, and whiteness 87%, the rate of recovery >=99.8%, water is not
Molten object 0.3%, purity 98.2%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method suitable for industrialized production high-purity sodium alginate, characterized in that the following steps are included:
(1) kelp sodium alginate extracting solution is subjected to micro-filtration clarification, obtains the clear sodium alginate extracting solution of yellowish-brown；
The clear condition of micro-filtration is: the aperture of ceramic micro filter film be 50~500nm, material liquid pH 8.0~9.0, feed liquid temperature 35~
45 DEG C, 0.15~0.4MPa of operating pressure, the water washing and micro-filtration of gained trapped fluid 2~3 times of volumes of filtrate；
(2) CaCl that mass volume ratio is 15~20% is added in the clear sodium alginate extracting solution of yellowish-brown in step (1)2
Solution, CaCl2Addition quality be kelp material quality used 15~25%, being stirred continuously makes calcium alginate Precipitation,
CaCl is added230~60min is stood after solution to be made to precipitate aging；
(3) filtering calcium alginate suspension obtains calcium alginate solid；
(4) light yellow calcium alginate solid is obtained using high concentration ethanol washing decoloration to the calcium alginate after separation of solid and liquid；
(5) the light yellow calcium alginate through high concentration ethanol washing decoloration is utilized into pure water washing；
(6) sodium alginate is converted for gained calcium alginate using ion-exchange, separation of solid and liquid obtains high saliferous sodium alginate
Solid；
(7) obtained high saliferous sodium alginate solid is dissolved in pure water, desalination and concentration by ultrafiltration obtains yellowish alginic acid
Sodium concentrate solution；
(8) ethyl alcohol to setting concentration is added into obtained yellowish sodium alginate concentrate solution further to decolourize and precipitate seaweed
Sour sodium, the final concentration of volume ratio 20~35% of the addition ethyl alcohol, is washed using the ethanol solution of same concentrations after separation of solid and liquid
Sodium alginate is washed, high-purity sodium alginate solid is obtained；
(9) dry to obtained above-mentioned sodium alginate and crush, obtain the sodium alginate product of high-purity.
2. preparation method as described in claim 1, it is characterized in that: kelp sodium alginate extracting solution contains water not in step (1)
Dissolubility particle, water soluble polymer, soluble small molecular and water-soluble inorganic salt；
Wherein, the water insoluble microparticle includes cell fragment, undissolved alginic acid, flocculate albumen and insoluble pigment, described
Water soluble polymer includes fucoidin, pectin, water-solubility protein and water colo(u)r, and soluble small molecular includes oligosaccharides, list
Sugar, mannitol and amino acid.
3. preparation method as described in claim 1, it is characterized in that: the operating condition of the filtering is: filter cloth in step (3)
Aperture is 200~400 mesh, and water washing 2~3 times of 2~3 times are added in gained filter cake, and gained greenish yellow solid filter cake is alginic acid
Calcium, separation of the resulting whole filtrate for kelp high added value functional components fucoidin and microelement is pure after mixing
Change.
4. preparation method as described in claim 1, it is characterized in that: the condition of ethanol decolorization is in step (4): high concentration second
The final concentration of volume ratio 65~85% of alcohol, bleaching temperature be 35~50 DEG C, bleaching time be 30~90min, decolorization 1~
3 times, obtain light yellow calcium alginate solid.
5. preparation method as described in claim 1, it is characterized in that: the condition of the ion exchange is: seaweed in step (6)
Sour calcium phase is that 5~10% are accounted for mass volume ratio for the additive amount of NaCl solution volume, and NaCl concentration is mass volume ratio 15
~20%, pH are 6.0~7.5, and switching architecture temperature is 35~55 DEG C, 20~60min of swap time, speed of agitator 100~
300r/min, calcium alginate not soluble in water are changed into soluble sodium alginate by ion exchange.
6. preparation method as described in claim 1, it is characterized in that: in step (7), the specific item of the desalination and concentration by ultrafiltration
Part: ultrafiltration retaining molecular weight is 1000~5000Da, 30~38 DEG C of temperature of charge, 0.15~0.5MPa of operating pressure, is extracted
Liquid cycles of concentration is 5~10 times, and gained concentrate uses water washing 2~3 times of 3~5 times of volumes, so that desalination is complete.
7. preparation method as described in claim 1, it is characterized in that: in step (8), the precipitate and decolorization time of the addition ethyl alcohol
For 30~120min, system temperature is 25~35 DEG C；Described be separated by solid-liquid separation uses flame filter press, and the aperture of filter cloth is 300~
500 mesh.
8. preparation method as described in claim 1, it is characterized in that: drying condition is 70~90 DEG C, when dry in step (9)
Between be 2~4h.
9. the high-purity sodium alginate product being prepared using method according to any one of claims 1 to 8, feature
Be: gained high-purity sodium alginate product is off-white color to white, whiteness > 85%, average recovery rate >=98%, water-insoluble
< 0.3%, purity 98-99.5%.
10. application of the method according to any one of claims 1 to 8 in industrialized production high-purity sodium alginate product.
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