CN108329402A - A method of digestion brown alga rhizome extracts algin - Google Patents
A method of digestion brown alga rhizome extracts algin Download PDFInfo
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- CN108329402A CN108329402A CN201710042247.3A CN201710042247A CN108329402A CN 108329402 A CN108329402 A CN 108329402A CN 201710042247 A CN201710042247 A CN 201710042247A CN 108329402 A CN108329402 A CN 108329402A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention belongs to seaweed chemical technical fields, and in particular to a method of digestion brown alga rhizome extracts algin.The method of the digestion brown alga rhizome extraction algin of the present invention, includes the following steps：1) pressure rolling：By the base portion of brown alga, stem and/or root pressure rolling to compression ratio 1.2~10；2) it impregnates：Add the brown alga after water submerged pressure rolling, 2~8h of soaking time；3) it digests：Soaked brown alga is subjected to alkaline process digestion and obtains digestive juice；4) product is obtained：It handles digestive juice and obtains algin.The present invention is by the base portion of brown alga, stem or root pressure rolling to there is crack, moisture can rapidly enter crack, and then continue to make to raw material internal penetration the immersion efficiency of the base portion of dry brown alga, stem (handle) or root to improve from crack, soaking time is greatly shortened.
Description
Technical field
The invention belongs to seaweed chemical technical fields, and in particular to a kind of side digesting extraction algin using brown alga as raw material
Method, especially a kind of method for digesting brown alga rhizome extraction algin.
Background technology
Algin is the general designation of alginic acid and its salt, a kind of plant polyose being present in brown algae plant, has thickening
Property, increase stability, emulsibility, pseudoplastic behavior, retentiveness, film forming and caking property, be widely used in food, textile printing and dyeing, medical treatment
The fields such as health, daily use chemicals, biotechnology and wastewater treatment.
Traditionally, industrially the primary raw material of extraction algin is Larminaria (Laminaria), Sargassum
(Sargassum), yellow tang category (Ascophyllum), Macrocystis (Macrocystis) this four class loadings short texture it is brown
Algae.Since fresh algae is difficult to store, general industry produces and uses dry algae raw material, and production technology continues to use traditional dry kelp algin
Production method, basic technology route include mainly impregnating, cutting the dish, digesting, is slag-liquid separation (rushing dilute, coarse filtration, floating and refined filtration), brown
Phycocolloid is precipitated (calcium is heavy), further carries out corresponding chemical conversion (acid cure, neutralization) to the algin of precipitation, obtains target brown alga
Hydrochlorate dries to obtain product.In addition, according to can increase before and after immersion the case where raw material washing, removal of impurities and etc..It can also basis
Raw material pigment etc. forms the color and luster requirement of situation and product, and fixation is carried out with formaldehyde or glutaraldehyde etc. to improve production before digestion
The color fixing agent such as formaldehyde are generally added using synchronous fixation is impregnated in existing industrial production in product color and luster that is, in soaking process,
It can be needed that fixation step progress substep fixation is separately provided before or after immersion according to production.If raw material is fresh algae, can save
Slightly impregnate.Wherein, digestion is the core of algin production technology, and digestion effect directly affects the yield of algin product and glues
Degree.
Since industrial brown alga raw material is mainly dry algae, in the technology of traditional digestion brown alga extraction algin, generally with
The pre-treatment step for impregnating and cutting the dish as digestion step, immersion in existing production technology cut the dish, digest and be classified as digestion techniques
Three processes, so that water is immersed frond in advance by impregnating, reduce frond size into passing through to cut the dish in order to disappearing convenient for digestion
Change the solid-liquid mixing in equipment.By taking the production of sodium alginate as an example, at present industrially using above-mentioned four kinds of brown algas as raw material, when immersion
Between generally 3~6h, digestion time is 3~6h, and (it is dry to raw material that yield refers to sodium alginate to the yield of the sodium alginate extracted
The yield of algae weight, similarly hereinafter；The dry algae refers to 15% algae raw material below of moisture content) it is generally 20~30g/100g, yield is
50%~70%, product viscosity (sodium alginate aqueous solution for referring to 1%) range of sodium alginate is generally 400~700mPas.
The brown algas raw materials such as above-mentioned traditional kelp, although (thickness or minor axis are generally little with relatively thin leaf or thinner stem
In 3.5mm) based on, but the thick stem (or handle) and root of compact structure (root shape object, holdfast) also occupy certain proportion, even if right
In the brown alga that kelp etc. breaks up without apparent base of leaf, thicker thallophytic base portion (part that thallus is connected with handle), handle and
The gross mass of root shape object generally may be up to the 6%~12% of kelp siccative gross mass.Inventor is using traditional kelp as raw material
It being found during digestion extraction algin, the leaf central part of kelp or the leaf portion of yellow tang have generally been soaked when impregnating 3h,
After digestion, leaf or thin stem have been resolved slagging (Fig. 1)；And thicker base portion, handle or root shape object etc. is still in bulk after digestion
Shape, and be not yet impregnated with (Fig. 2 and 3) by reaction solution.It can be seen that base portion, stem (handle) or root (root shape that structure is comparatively dense
Object, holdfast) immersion efficiency (Liquid Penetrant efficiency) and digestive efficiency lag far behind relatively thin leaf portion or thin stem, this part
Most of algin in raw material is difficult to be converted dissolution in digestion process.According to document, (Chen Limei, Li Demao etc., kelp is not
It is studied with position algin content and its gelling performance, Food Additives Used in China, 2010 (02):124-126+142.) report, sea
Algin content with thallus base portion between thallophytic middle part and the algin content of tip, so, the base of kelp
Algin content in portion, stem (handle) or root (root shape object, holdfast) also can not be ignored.However, being carried using existing digestion
Take technology, the Liquid Penetrant efficiency of thicker base portion, stem (handle) or root (root shape object, holdfast) lag far behind it is thallophytic in
Portion and tip cannot still be permeated after digestion reaction by reaction solution, and internal algin is it is even more impossible to be extracted, Shi Bizao
At the waste of resource.Therefore, the digestive efficiency for improving base portion, stem (handle) or root (root shape object, holdfast) is former to improving tradition
The yield of material algin is of great significance.
In recent years, above-mentioned traditional raw material is gradually developed as food or high-grade feed, price go up year by year, and manufacturing enterprise opens
Beginning seeks other type brown algas of inedibility as raw material.Thunder pine Trentepohlia (Lessonia) has apparent leaf, stem differentiation (with stem
Based on), stem structure is fine and close, quality is hard, it is difficult to digest, inedibility, algin content, can higher than traditional raw materials such as kelps
Reach 40~45g/100g raw materials, the Lei Songzao of compact structure becomes a kind of raw material selection of extraction algin.Thunder in the market
Generally from the dry algae bulk cargo of Chile or Peru's import, (moisture content is generally the raw material of 13%~18%, Lei Songzao to loose algae raw material
Weight or dry algae weight are in terms of the thunder pine algae raw material of moisture content 15%), with the stem of 5~20mm of diameter, 10~50mm of length in raw material
Based on (the more difficult differentiation of stem and root, is referred to as with stem in bulk cargo), can generally account for 70% of gross weight or more.Document (swallow etc., mistake
Journey engineering journal, 2016,16 (1)：144-150) using the process route of existing " impregnating-cutting the dish-to digest ", by screw thread thunder pine
The stem of algae (Lessonia trabeculata, one kind of thunder pine Trentepohlia) is at 35 DEG C in 2% formalin of 10 times of dry algae weights
1~3mm progress digestion reactions are crushed to after impregnating and (impregnating synchronous fixation) 48h in solution, have investigated Na2CO3Concentration (1%~
2.33%), feed liquid mass ratio (1:10~1:20), speed of agitator (100~400r/min), digestion temperature and disappear at (60~90 DEG C)
Change influence of the time (6~10h) to algin digestion yield and alginate solution viscosity, by orthogonal experiment to digestion process item
Part optimizes, and the best digestion condition determined is：Temperature 70 C, Na2CO3Concentration 1.67%, speed of agitator 400r/min, material
Liquid mass ratio 1:15, digestion time 8h.The product yield of sodium alginate is 34.80g/100g under this condition, and product viscosity is
2261.67mPas far above the 173.30mPas of commercial product.But the soaking time of screw thread thunder pine algae is extended for
As many as 8 times of 48h, about traditional raw material (3~6h)；Even if the screw thread thunder pine algae for impregnating 48h is crushed to 1~3mm, it is still necessary to disappear
Change 8h, just the yield of algin can be made to reach 30g/100g or more, the digestion time (about 3~6h) than traditional raw material increases to
Few 2h.Traditional digestion extraction process is for the thunder pine algae digestion extraction algin based on stem, soaking time and digestion time
Substantially extend, production efficiency is by serious restriction.Thunder pine algae stem is impregnated discovery by inventor at 35 DEG C, even if will impregnate
Time lengthening is not also soaked (Fig. 4) to 48h, Lei Songzao.It can be seen that document (swallow etc., process engineering journal, 2016,
16(1)：144-150) the thunder pine algae for being used for digestion is the Lei Songzao not soaked, and digestion process is actually to be soaked in digestion
Bubble, therefore, digests even if the thunder pine algae for impregnating 48h is crushed to 1~3mm, 8h is still needed under best digestion condition, digests
Efficiency is longer than the digestion time of traditional raw material far below raw materials, digestions time such as traditional kelps.
To sum up, extractive technique is digested using existing algin, it is thicker for the brown algas raw material such as traditional kelp
Base portion, the immersion efficiency of thick stem (handle) or root shape object and digestive efficiency lag far behind leaf or thin stem, make big in this part material
Part algin can not be converted extraction, cause the waste of resource；For the Lei Songzao based on the stem with compact structure,
It is even more to further decrease to impregnate efficiency and digestive efficiency, and soaking time and digestion time are longer than the brown algas such as traditional kelp original
Material, production efficiency is by serious influence.
Invention content
During the present invention is directed to using brown alga as raw material digestion extraction algin, by stem (handle) or root (root shape object, fixation
Device) the impermeable and thus low problem of caused digestive efficiency is impregnated caused by compact structure, a kind of digestion brown alga rhizome is provided and is carried
The method for taking algin, the rhizome (raw material) include the base portion of brown alga, stem (handle) or root (root shape object, holdfast), or, with
Brown alga based on stem and root.
The present invention digestion brown alga rhizome extraction algin method, existing production process route soaking step it
Before, increase the step of pressure rolling is carried out to brown alga rhizome, by the base portion of brown alga, stem or root pressure rolling to crack occur but not broken open.
Specifically, being compressed to 20~350MPa of compression ratio 1.2~10 or pressure.Wherein, the compression ratio is pressure rolling on compression direction
Diameter ratio after preceding diameter and pressure rolling, the pressure are the pressure of algae block unit forced area.
For the present invention by the base portion of brown alga, stem or root pressure rolling to there is crack, moisture can rapidly enter crack, and then from splitting
Continue to be equivalent to the practical seepage distance for shortening moisture or reaction solution to raw material internal penetration at seam, make dry brown alga base portion,
The immersion efficiency of stem (handle) or root improves, and soaking time is greatly shortened；Immersion, which fully makes to form inside raw material, well fills
The moisture distribution divided provides for the dissolving diffusion of the conversion reaction of the algin of digestion step, reaction reagent and target product
Good water environment makes the base portion, stem (handle) or the digestive efficiency of root of brown alga significantly improve, and shortens digestion time.
The specific implementation mode of the present invention is as follows：
The method of the digestion brown alga rhizome extraction algin of the present invention, includes the following steps：
1) pressure rolling：By the base portion of brown alga, stem and/or root pressure rolling to compression ratio 1.2~10；
2) it impregnates：Add the brown alga after water submerged pressure rolling, 2~8h of soaking time；
3) it digests：Soaked brown alga is subjected to alkaline process digestion and obtains digestive juice；
4) product is obtained：It handles digestive juice and obtains algin.
Method according to the present invention, wherein the step 2) amount of water is brown alga weight (to be converted into moisture content
The weight meter of 15% dry algae, similarly hereinafter) 7~15 times, 20~35 DEG C of the soaking temperature.In step 3) the alkaline process digestion,
Water consumption is 10~30 times of brown alga weight, and sodium carbonate amount is the 15%~40% of brown alga weight.
Method according to the present invention, wherein preferably, in step 3) the alkaline process digestion, digestion temperature is 60~85
DEG C, 3~6h of digestion time.
Method according to the present invention, in the step 3) " digestion ", soda ash can be added with solid forms, also may be used
With Na2CO3Aqueous solution form is added, and can be added at one time, and the mode that stream adds or segmentation is added can also be used；Water can disposably add
Enter, the mode that stream adds or segmentation is added can also be used and be added.
Method according to the present invention, the subsequent processing of gained digestive juice can refer to prior art and carry out corresponding algin
The production of product such as carries out slag-liquid separation acquisition clear glue solution by prior art, makes calcium alginate from clear glue solution by the calcium method of sinking
It is precipitated, is corresponding brown by the processes production such as hydrochloric acid decalcification acquisition alginic acid and neutralized conversion acquisition target alginate
Alginates also can carry out corresponding subsequent technique improvement and design according to the actual needs and requirement of production.
Method according to the present invention, wherein step 1) the pressure rolling method includes roll-in, squeezing, squeezes and roll
One or more of Deng, it is preferable that using roller press types equipment such as roll squeezer, double-roll crusher, multiple roll crushers.
Method according to the present invention, preferably, the pressure rolling described in step 1) make algae block by 20~350MPa
Between pressure effect, realize needed for compression ratio 1.2~10.0.
Method according to the present invention, wherein the brown alga includes but not limited to Larminaria (Laminaria), horse hair
Trentepohlia (Sargassum), yellow tang category (Ascophyllum), Macrocystis (Macrocystis), kelp category (Ecklonia), face
The one or more of algae in Trentepohlia (Tinocladia) and thunder pine Trentepohlia (Lessonia).It is preferred that Larminaria
(Laminaria) Sargassum (Sargassum of kelp (Laminaria japonica), Sargassum (Sargassum)
Pallidum), the bulk kelp of the yellow tang (Ascophyllum nodosum), Macrocystis of yellow tang category (Ascophyllum)
The noodles algae of bark algae (Ecklonia maxima), noodles Trentepohlia that (Macrocystis pyrifera), kelp belong to
In (Tinocladia crassa (Sur.) Kuck.) and the screw thread thunder pine algae (Lessonia trabeculata) of thunder pine Trentepohlia
One or more.
Method according to the present invention, wherein can according to the impurity situation of raw material, before the step 1) pressure rolling or
The step of increasing washing or removal of impurities later.
Method according to the present invention, wherein sorting step can also be increased before the step 1) pressure rolling, by root
And/or stem is detached with leaf.Specifically, root that can be according to raw material, stem content situation increase the step of sorting before step 1) pressure rolling
Suddenly, root, stem are detached with leaf, or improve step 1) raw material in root, stem content.The sorting step is being washed or is being removed
Before miscellaneous step.
Method according to the present invention, wherein one kind as the present invention is preferably, the pressure rolling described in step 1) can be to original
It is about 1.5~3.3 that material carries out pressure rolling to compression ratio respectively after being classified according to diameter, be more than 5mm according to diameter but be less than etc.
In 10mm, diameter is more than 10mm but is less than or equal to 20mm, and diameter is more than 20mm, is divided into three grades, carries out pressure rolling respectively.
Method according to the present invention, wherein one kind as the present invention is preferably, the pressure rolling described in step 1) can will be brown
It is 1.7~2.5 that pressure rolling to compression ratio is carried out after algae feedstock processing to moisture content 13%~20%, preferably, using pressure
70~160MPa carries out pressure rolling, realizes required compression ratio.
Method according to the present invention, wherein as an improvement of the present invention, can increase before step 3) " digestion "
Add fixation step, to reduce dissolution of the impurity such as pigment in digestion process, improves product color, the condition of fixation step can join
According to the color fixing condition of prior art.Specifically, individual fixation step can be increased before step 2) " immersion ", or in step 2)
It is synchronous during " immersion " to carry out fixation, it can also increase individual fixation step between step 2) " immersion " and step 3) " digestion "
Suddenly.The color fixing agent dosage is the 5%~15% of brown alga weight, the 5%~15% of most preferably dry algae weight.The color fixing agent can
To use all kinds of color fixing agent, such as formaldehyde, glutaraldehyde well known in the art etc., the present invention is not limited.
Method according to the present invention, wherein described in the step 3) " digestion " can selectively add 1% in the process~
The crosslinking agents such as the formaldehyde or glutaraldehyde of 10% dry algae weight, further increase the viscosity of algin product.
Method according to the present invention, wherein the digestion method of " boil in a covered pot over a slow fire-stirring " can be used in the step (3) " digestion ",
Or, using the method that " boil in a covered pot over a slow fire-stirring " is combined with defibrination (for example, " boil in a covered pot over a slow fire-being stirred " disclosed in patent CN101585890B and " jordan mill
It is broken " combine three-level digestion：" boil in a covered pot over a slow fire-stirring "-" jordan is ground "-" boil in a covered pot over a slow fire-stirring "-" jordan is carried out to the bulk kelp impregnated and shredded
Grind " the digestion of-three-level of " boil in a covered pot over a slow fire-stirring "), or, using continuously stirring or continuously stirring the method combined with " defibrination ".Preferably,
Using the digestion method continuously stirred.
Method according to the present invention as an improvement of the present invention can be after the step 2) " immersion "
The step of increasing " wet algae crushes ".Described " the wet algae crushes " step can be before or after independent increased fixation step.
" wet algae crushes " is that the brown alga after impregnating is crushed to average size granularity d50For 1.5~3mm.
The technical characterstic of the present invention is as follows：
It is soaked, in digestion process for positions difficulties such as base portion, stem and roots in the brown alga or brown alga based on stem and root class
The problem of soaking time is long caused by the infiltration of reaction solution difficulty, digestion rate is slow, brown alga glue yield is low, the wasting of resources, improves raw material
Liquid-solid mass transfer performance, impregnate efficiency and digestive efficiency to improve.
(1) inventor compresses it the study found that since the base portion, stem or root of brown alga are with certain toughness to pressure
Ratio contract between 1.2~10, preferably makes it by the pressure between 20~350MPa when acting on, the stem (handle) of brown alga or root
Surface (Fig. 5) and internal (Fig. 6) can generate crack, but size degradation not will produce disintegrating slag and dust at fritter.
(2) present invention makes the base portion, stem (handle) and root of brown alga crack occur, moisture can by the way that brown alga is carried out pressure rolling
Rapidly enter crack, then to raw material internal penetration from crack, be equivalent to shorten the practical infiltration of moisture or reaction solution away from
From making the base portion, stem (handle) or the immersion efficiency of root of dry brown alga significantly improve (Fig. 7-10).
(3) by soaking at the positions such as stem, root in brown alga in advance, by inefficient moisture penetration process from digestion process
In the step of being stripped out, " cutting the dish " can be omitted, improve digestive efficiency, shorten digestion time.
The present invention having the beneficial effect that compared with prior art：
By before soaking step increase to brown alga carry out pressure rolling the step of, for traditional raw material (kelp, sargassum,
Yellow tang, bulk kelp), can make thicker base portion, stem (handle) and root (root shape object, holdfast) reach immersion identical with leaf portion and
Digestive efficiency improves the yield of algin；For brown alga (thunderous pine algae) raw material based on the stem and root with compact structure, impregnate
Time is foreshortened to by 48h in 8h, and digestion time can foreshorten within 6h, and it is brown that algin product yield can reach 25~38g/100g
Algae (in terms of the weight of dry algae for being converted into moisture content 15%, similarly hereinafter), yield can reach 60%~90%, reach and traditional raw material
Comparable immersion efficiency and digestive efficiency, 42h or more can be shortened with the time of two processes of digestion by impregnating；It in addition can before digestion
Omission is cut the dish step.
On the other hand, for the Lei Songzao of compact structure, increase the step of pressure rolling is carried out to brown alga, impregnate efficiency and digestion
Quite with traditional raw material (kelp, sargassum, yellow tang, bulk kelp), soaking time and digestion time are consistent with traditional raw material for efficiency,
Soaking conditions identical with traditional raw material can be set, and the digestion process condition close with traditional raw material is production operation and management
It provides a convenient.
Description of the drawings
Fig. 1 is the filtrate after kelp digestive juice coarse filtration.
Fig. 2 is the algae block residual after kelp digestive juice coarse filtration.
Fig. 3 is the reaction solution of remaining handle and root shape object infiltration situation after kelp digestive juice coarse filtration.
Fig. 4 is the moisture penetration situation that untreated thunder pine algae stem impregnates different time, in figure for after impregnating in an axial direction
Section.
Fig. 5 is the photo of thunder pine algae stem.Wherein, (a) is the photo of untreated Lei Song algaes stem；(b) it is radially
Lei Song algaes stem photo；(c) it is the photo of Lei Song algaes stem in an axial direction.
Fig. 6 is the microscope photo of thunder pine algae stem slice.Wherein, (a)：Untreated thunder pine algae stem slice；(b)：Pressure
The rear internal thunder pine algae stem slice for generating gap is rolled, white gaps therein are cracks.
Fig. 7 impregnates the moisture penetration situation of 6h for the thunder pine algae stem of (compression ratio 2) after pressure rolling, wherein soak is red
Ink solution, section are section both axially and radially.
Fig. 8 impregnates the moisture penetration situation of 6h for the thunder pine algae stem of (compression ratio 2) after pressure rolling, wherein soak is certainly
Water, section are section in an axial direction.
Fig. 9 impregnates the moisture penetration situation of 6h for the thunder pine algae stem of (compression ratio 2) after pressure rolling, wherein soak is certainly
Water, section are section radially.
Figure 10 is that water absorption rate changes with time in the untreated thunder pine algae stem soaking process with after pressure rolling.It is therein
" pressure " is the pressure of algae block unit forced area.
Figure 11 is the yield of the sodium alginate product under different digestions time in comparative example 1.
Figure 12 is the yield of the sodium alginate product under different digestions time in comparative example 3.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
Algin is extracted using the digestion process route of this technology, raw material is screw thread thunder pine algae (Lessonia
Trabeculata), the diameter range of thunder pine algae stem is about 5~20mm, originates from Chile, is purchased from Runlin investment
co.,LTD。
(1) pressure rolling：By two roller gap adjustments of double-roll crusher to about 5mm, 1t screw thread thunder pine algaes are broken by two pairs of rollers
It is about 1.2~5 that broken machine, which is depressed into compression ratio, and the diameter range of thunder pine algae is about 5~20mm before compressing, along pressure rolling direction after compression
Diameter range is about 4~5.5mm.
(2) it impregnates：At 20 DEG C, in 10m32h is impregnated in the tap water of (about 10 times of dry algae weights).
(3) it digests：Digestion pot is added in soaked thunder pine algae, 10m is added360 ± 5 DEG C of the heat of (10 times of dry algae weights)
Water is added the sodium carbonate of 150kg (15% dry algae weight), digestion is kept the temperature at 60 DEG C, is boiled in a covered pot over a slow fire 45 minutes, 15min is stirred, digests 3h,
Obtain digestive juice.
The subsequent processing of gained digestive juice carries out the production of sodium alginate product with reference to prior art, specific as follows：To disappearing
Change the tap water thinning that 100 times of dry algae weights are added in liquid, opens 6 mesh filters and carry out coarse filtration, filtrate is injected in floating pool and is floated
Sieve refined filtration of the glue after floating through 120~200 mesh is obtained clear glue solution by floating 3h；After clear glue solution is adjusted to pH=6.5,
The calcium chloride solution of mass concentration 12% is added, calcium ion concentration in calcification tank is made to pass through between 0.045%~0.050%
Calcium is heavy to obtain calcium alginate；Calcium alginate is put into decalcification tank, after adding water to submerge calcium alginate, the salt of mass fraction 31% is added
Acid obtains alginic acid to pH=2, decalcification about 2h；Alginic acid is dehydrated to water content less than after 70% using pressafiner, powder
After broken and the alcohol of concentration 90% presses 1:1 ratio puts into neutralizing tank together, and the hydrogen-oxygen that mass concentration is 40% is added while stirring
Change sodium solution, pH is made to maintain 8 or so, until pH constant；Sodium alginate is dried to moisture content after separation of solid and liquid and is less than 15%,
Obtain sodium alginate 250kg, yield be 25.0g/100g brown algas (in terms of the weight of dry algae for being converted into moisture content 15%, under
Together), the viscosity of 1% sodium alginate aqueous solution is 1176mPas.
Embodiment 2
Algin is extracted using the digestion process route of this technology, other are with embodiment 1, the difference is that by double-roll crusher
Roller spacing be adjusted to 2mm, it is 2.5~10 that thunder pine algae stem, which is depressed into compression ratio, and final to obtain sodium alginate 262kg, yield is
The viscosity of 26.2g/100g brown algas, 1% sodium alginate aqueous solution is 1165mPas.
Embodiment 3
Algin is extracted using the digestion process route of this technology, other are with embodiment 1, the difference is that roll squeezer is used,
The pressure (compression) that thunder pine algae stem is subject to is set to be about 20MPa, it is about 1.2 that thunder pine algae stem, which is depressed into compression ratio, is finally obtained brown
Mosanom 170kg, yield are 17.0g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is 1345mPas.
Embodiment 4
Algin is extracted using the digestion process route of this technology, other with embodiment 3, unlike make thunder pine algae stem by
The pressure (compression) arrived is 350MPa, and it is about 10 that thunder pine algae stem, which is depressed into compression ratio, final to obtain sodium alginate 280kg, is obtained
Rate is 28.0g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is 1327mPas.
Embodiment 5
Algin is extracted using the digestion process route of this technology, other with embodiment 3, unlike make thunder pine algae stem by
The pressure (compression) arrived is 200MPa, and it is about 2.54 that thunder pine algae stem, which is depressed into compression ratio, final to obtain sodium alginate 247kg,
Yield is 24.7g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is 1225mPas.
Embodiment 6
Algin is extracted using the digestion process route of this technology, other are with embodiment 5, the difference is that soaking time is
8h, final to obtain sodium alginate 251kg, yield is 25.1g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
1372mPa·s。
Embodiment 7
Algin is extracted using the digestion process route of this technology, other are with embodiment 5, the difference is that soaking time is
5h, final to obtain sodium alginate 250kg, yield is 25.0g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
1372mPa·s。
Embodiment 8
Algin is extracted using the digestion process route of this technology, other are with embodiment 7, the difference is that digestion temperature is 80
DEG C, final to obtain sodium alginate 262kg, yield is 26.2g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
1267mPa·s。
Embodiment 9
Algin is extracted using the digestion process route of this technology, other are with embodiment 7, the difference is that digestion temperature is 70
DEG C, final to obtain sodium alginate 257kg, yield is 25.7g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
1191mPa·s。
Embodiment 10
Algin is extracted using the digestion process route of this technology, Fresh Laminaria Japonica (Laminaria japonica) (is contained
Water rate is about root 88%) and handle uses pressure 100MPa to carry out pressure rolling to compression ratio as 1.2, other are different with embodiment 7
It is that digestion water consumption is heavy for 40 times of dry algaes, final to obtain sodium alginate 37.4kg, yield is 26.5g/100g brown algas, 1% brown alga
The viscosity of acid sodium aqueous solution is 1137mPas.
Embodiment 11
Algin is extracted using the digestion process route of this technology, Fresh Laminaria Japonica (Laminaria japonica) (is contained
Water rate is about 88%) to dry to moisture content 15%, and the kelp after taking 1t to dry carries out pressure rolling using pressure 70MPa, makes kelp
Root and the compression ratio of handle be about 1.7, other with embodiment 7, unlike digestion water consumption be 40 times of dry algaes weights, it is final to obtain
Sodium alginate 295kg, yield are 29.5g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is 1137mPas.
Embodiment 12
Algin is extracted using the digestion process route of this technology, by the dry kelps of 1t (moisture content 13%) plus water damping to containing
Pressure rolling is carried out using pressure 160MPa after water rate 20%, the compression ratio of the root and handle that make kelp is about 2.5, other with embodiment 7,
Unlike digestion water consumption be 15 times of dry algaes weights, final to obtain sodium alginate 315kg, yield is 30.8g/100g brown algas, 1%
The viscosity of sodium alginate aqueous solution is 1221mPas.
Embodiment 13
Algin is extracted using the digestion process route of this technology, other are with embodiment 7, the difference is that sodium carbonate amount is
The 40% of dry algae weight obtains sodium alginate 267kg, and yield is 26.7g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
1115mPa·s。
Embodiment 14
Algin is extracted using the digestion process route of this technology, other are with embodiment 7, the difference is that sodium carbonate amount is
The 25% of dry algae weight obtains sodium alginate 247kg, and yield is 24.7g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
1227mPa·s。
Embodiment 15
Algin is extracted using the digestion process route of this technology, other are with embodiment 14, the difference is that digestion time is
6h obtains sodium alginate 323kg, and yield is 32.3g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is 1415mPa
s。
Embodiment 16
Algin is extracted using the digestion process route of this technology, other are with embodiment 15, the difference is that thunder pine algae is pressed
Pressure rolling is carried out using oppositely rolling roller crusher after being classified according to diameter, diameter is more than 5mm but less than or equal to 10mm, uses
Roller spacing is 3mm, and diameter is more than 10mm but uses roller spacing for 6mm less than or equal to 20mm, and diameter uses roller more than 20mm's
Spacing is 11mm, is divided into three grades, between progress pressure rolling to compression ratio is about 1.5~3.3 respectively, obtains sodium alginate
321kg, yield are 32.1g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is 1371mPas.
Embodiment 17
Algin is extracted using the digestion process route of this technology, other are with embodiment 15, the difference is that raw material thunder pine
It is 20% that algae watering damping, which is moisture content, and diameter is more than 5mm but less than or equal to 10mm, uses roller spacing for 3mm, diameter is more than
10mm but use roller spacing for 6mm less than or equal to 20mm, what diameter was more than 20mm uses roller spacing for 11mm, is divided into three etc.
Grade between progress pressure rolling to compression ratio is about 1.5~3.3 respectively, obtains sodium alginate 321kg, and yield is that 32.1g/100g is brown
The viscosity of algae, 1% sodium alginate aqueous solution is 1379mPas.
Embodiment 18
Algin is extracted using the digestion process route of this technology, other with embodiment 15, unlike digestion method by
45 minutes stewing, stirring 15min, is changed into and continuously stirs, and digestion 6h obtains sodium alginate 330kg, and yield is that 33.0g/100g is brown
The viscosity of algae, 1% sodium alginate aqueous solution is 1357mPas.
Embodiment 19
Algin is extracted using the digestion process route of this technology, other are with embodiment 15, the difference is that initial impregnating
The formaldehyde of 10% dry algae weight is added into soaking water, sodium alginate 331kg is obtained when digesting 6h, yield is that 33.1g/100g is brown
The viscosity of algae, 1% sodium alginate aqueous solution is 2217mPas, and color and luster is faint yellow.
Embodiment 20
Algin is extracted using the digestion process route of this technology, other with embodiment 15, unlike it is initial in digestion,
The formaldehyde of 5% dry algae weight is added into digestion pot, digestion 6h obtains sodium alginate 333kg, and yield is 33.3g/100g brown algas,
The viscosity of 1% sodium alginate aqueous solution is 2615mPas.
Embodiment 21
Algin is extracted using the digestion process route of this technology, other are with embodiment 15, the difference is that after dipping
Brown alga is crushed to d50=2mm, obtains sodium alginate 384kg, and yield is 38.4g/100g brown algas, 1% sodium alginate aqueous solution
Viscosity be 1335mPas.
Embodiment 22
Algin is extracted using the digestion process route of this technology, other are with embodiment 20, the difference is that initial impregnating
The formaldehyde of 10% dry algae weight is added into soaking water, sodium alginate 376kg is obtained when digesting 6h, yield is that 37.6g/100g is brown
The viscosity of algae, 1% sodium alginate aqueous solution is 2317mPas, and color and luster is faint yellow, pH=7.05.
Comparative example 1
Algin is extracted using the digestion process route of " immersion-crushing-digestion ", raw material is with embodiment 1, by screw thread thunder pine
After algae impregnates 8h at 20 DEG C in the tap water of 10 times of dry algae weights, it is crushed to d50=6.5mm (3~10mm of particle size range) is carried out
With embodiment 13, carrying out processing obtains sodium alginate after a certain period of time, to digestive juice for digestion, right for digestion, digestion and process conditions
The subsequent processing of digestive juice is shown in Figure 11 with embodiment 1, the yield of the sodium alginate product obtained under different digestions time, is disappearing
When the change time reaches 10h, the yield of sodium alginate product is 15.0g/100g brown algas, and the viscosity of 1% sodium alginate aqueous solution is
365mPa·s。
Comparative example 2
Algin is extracted using the digestion process route of " immersion-crushing-digestion ", other are with comparative example 1, the difference is that will
Screw thread thunder pine algae at 20 DEG C in the tap water of 10 times of dry algae weights after immersion 8h is crushed to d50=2mm (particle size range 1~
It 3mm) is digested, the product yield for digesting the sodium alginate of 8h is 25.0g/100g brown algas, and 1% sodium alginate aqueous solution glues
Degree is 710mPas.
Comparative example 3
Algin is extracted using the digestion process route of " immersion-crushing-digestion ", other are with comparative example 1, the difference is that will
Screw thread thunder pine algae is crushed to after impregnating and (impregnating synchronous fixation) 48h in 2% formalin of 10 times of dry algae weights at 35 DEG C
d50=2mm (1~3mm of particle size range) is digested, and carrying out processing obtains sodium alginate after a certain period of time, to digestive juice for digestion,
The yield of sodium alginate product under different digestions time is shown in Figure 12.Digestion 8h obtain sodium alginate product yield be
The viscosity of 34.4g/100g brown algas, 1% sodium alginate aqueous solution is 2160mPas, but soaking time and digestion time are notable
It is longer than traditional raw material, cannot be arranged production using existing production routine.
Certainly, the present invention can also there are many embodiments, without deviating from the spirit and substance of the present invention, are familiar with
Those skilled in the art can disclosure according to the present invention make various corresponding change and deformations, but these it is corresponding change and
Deformation should all belong to the scope of the claims of the present invention.
Claims (14)
1. a kind of method of digestion brown alga rhizome extraction algin, includes the following steps：
1) pressure rolling：By the base portion of brown alga, stem and/or root pressure rolling to compression ratio 1.2~10；
2) it impregnates：Add the brown alga after water submerged pressure rolling, 2~8h of soaking time；
3) it digests：Soaked brown alga is subjected to alkaline process digestion and obtains digestive juice；
4) product is obtained：It handles digestive juice and obtains algin.
2. according to the method described in claim 1, it is characterized in that, the step 2) amount of water is 7~15 times of brown alga weight,
20~35 DEG C of the soaking temperature；Wherein, the brown alga weight is the weight that brown alga is converted into the dry algae of moisture content 15% and is calculated
Amount.
3. according to the method described in claim 1, it is characterized in that, in step 3) the alkaline process digestion, water consumption is brown alga weight
10~30 times of amount, sodium carbonate amount are the 15%~40% of brown alga weight；Wherein, the brown alga weight is to be converted into brown alga
The weight that the dry algae of moisture content 15% calculates.
4. method according to claim 1 or 3, which is characterized in that in step 3) the alkaline process digestion, digestion temperature is 60
~85 DEG C, 3~6h of digestion time.
5. according to any methods of claim 1-4, which is characterized in that step 1) the pressure rolling method includes roll-in, pressure
One or more of squeeze, squeeze and roll.
6. according to any methods of claim 1-4, which is characterized in that carry out pressure rolling using 20~350MPa of pressure.
7. according to any methods of claim 1-4, which is characterized in that increase before or after the step 1) pressure rolling
The step of washing or removal of impurities.
8. according to any methods of claim 1-4, which is characterized in that increase sorting step before the step 1) pressure rolling
Suddenly, root and/or stem are detached with leaf.
9. according to any methods of claim 1-4, which is characterized in that step 1) by the base portion of the brown alga, stem and/or
It is about 1.5~3.3 that root carries out pressure rolling to compression ratio respectively after being classified according to diameter；Wherein, according to diameter be more than 5mm but
Less than or equal to 10mm, diameter is more than 10mm but is less than or equal to 20mm, and diameter is more than 20mm, is divided into three grades, is pressed respectively
It rolls.
10. according to any methods of claim 1-4, which is characterized in that step 1) handles brown alga to moisture content 13%
It is 1.7~2.5 that pressure rolling to compression ratio is carried out after~20%, it is preferable that carries out pressure rolling using 70~160MPa of pressure.
11. according to any methods of claim 1-4, which is characterized in that before step 2) immersion, or in step 2)
In soaking process, or after step 2) immersion, before step 3) digestion, color fixing agent is added and carries out fixation.
12. according to any methods of claim 1-4, which is characterized in that be added 1% in the step 3) digestion process
The formaldehyde or glutaraldehyde of~10% dry algae weight.
13. according to any methods of claim 1-4, which is characterized in that the step 3) digestion stirs combination using stewing
Digestion method, either using the stewing digestion method combined with defibrination that stirs either using the digestion method or use continuously stirred
Continuously stir the digestion method combined with defibrination.
14. according to any methods of claim 1-4, which is characterized in that step 2) increases wet algae pulverising step after impregnating.
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| CN102060938A (en) * | 2010-12-24 | 2011-05-18 | 青岛明月海藻集团有限公司 | Method for extracting algin through comprehensively utilizing brown algae |
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