CN108329402B - Method for extracting algin by digesting brown algae rhizome - Google Patents
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Abstract
The invention belongs to the technical field of seaweed chemical industry, and particularly relates to a method for extracting algin by digesting brown seaweed rhizomes. The method for extracting the algin by digesting the rhizomes of the brown algae comprises the following steps: 1) rolling: rolling the base, stem and/or root of the brown algae to a compression ratio of 1.2-10; 2) soaking: adding water to submerge the rolled brown algae, and soaking for 2-8 h; 3) digestion: performing alkaline digestion on the soaked brown algae to obtain a digestive juice; 4) obtaining a product: treating the digestive juice to obtain algin. The invention rolls the base, stem or root of the brown algae until cracks appear, and the water can quickly enter the cracks, so that the water can continuously permeate into the raw material from the cracks, thereby improving the soaking efficiency of the base, stem (stem) or root of the dry brown algae and greatly shortening the soaking time.
Description
Technical Field
The invention belongs to the technical field of seaweed chemical industry, and particularly relates to a method for digesting and extracting algin by taking brown algae as a raw material, in particular to a method for digesting and extracting algin from brown algae rhizomes.
Background
Algin is a generic name of alginic acid and salts thereof, is a plant polysaccharide existing in brown algae plants, has thickening property, stability, emulsifying property, pseudoplasticity, water retention property, film forming property and cohesiveness, and is widely applied to the fields of food, textile printing and dyeing, medical treatment and sanitation, daily use chemicals, biotechnology, wastewater treatment and the like.
Traditionally, the main raw materials for industrially extracting algin are four kinds of brown algae with loose tissue structures, i.e., Laminaria (Laminaria), Sargassum (Sargassum), Ascophyllum (Ascophyllum) and Macrocystis (Macrocystis). The production process mainly comprises the steps of soaking, cutting vegetables, digesting, separating residues and liquids (diluting, coarse filtering, floating and fine filtering), separating out the algin (calcium precipitation), further performing corresponding chemical conversion (acid coagulation and neutralization) on the separated algin to obtain target alginate, and drying to obtain the product. In addition, according to the condition of raw materials, steps of washing, impurity removal and the like can be added before and after soaking. The color of the product can be improved by fixing the color with formaldehyde or glutaraldehyde and the like before digestion according to the composition conditions of raw material pigments and the like and the color requirement of the product, and the prior industrial production generally adopts soaking synchronous color fixation, namely adding color fixing agents such as formaldehyde and the like in the soaking process, and also can independently set a color fixing step before or after soaking according to the production requirement to carry out color fixation step by step. If the raw material is fresh algae, soaking can be omitted. Wherein, digestion is the core of the production process of the algin, and the digestion effect directly influences the yield and the viscosity of the algin product.
Because the raw material of industrial brown algae is mainly dry algae, in the traditional technology for digesting brown algae to extract algin, soaking and cutting vegetables are generally taken as pretreatment steps of the digestion step, and soaking, cutting vegetables and digestion in the existing production process are divided into three procedures of the digestion technology. Taking the production of sodium alginate as an example, at present, the four kinds of brown algae are taken as raw materials industrially, the soaking time is generally 3-6 h, the digestion time is 3-6 h, the yield of the extracted sodium alginate (the yield refers to the yield of the sodium alginate to the weight of dry algae of the raw materials, the same is applied below; the dry algae refers to the algae raw materials with the water content of below 15%) is generally 20-30 g/100g, the yield is 50-70%, and the product viscosity of the sodium alginate (refers to 1% sodium alginate aqueous solution) is generally 400-700 mPas.
Although the above-mentioned conventional brown algae raw materials such as kelp and the like mainly comprise thin leaves or thin stems (thickness or short diameter is generally not more than 3.5mm), thick stems (or stalks) and roots (roots and fixers) with compact structures account for a certain proportion, and even for brown algae such as kelp and the like which do not have obvious stem differentiation, the total mass of the bases (parts where the fronds are connected with the stalks), the stalks and the roots of the thick fronds can generally be as high as 6-12% of the total mass of the dry kelp materials. The inventor discovers that the middle part of the leaves of the kelp or the leaf part of the Ascophyllum nodosum is soaked thoroughly when being soaked for 3 hours in the process of digesting and extracting the algin by taking the traditional kelp as a raw material, and the leaves or the thin stems are digested into dregs after digestion (figure 1); while the thicker base, stem or root etc. remain in large chunks after digestion and are not yet soaked by the reaction solution (fig. 2 and 3). Therefore, the soaking efficiency (liquid permeation efficiency) and the digestion efficiency of the base part, the stem (stalk) or the root (root-shaped object, fixator) with a compact structure are far lagged behind those of the thinner leaf part or thin stem part, and most of the algin in the raw material is difficult to be converted and dissolved out in the digestion process. According to the literature (Chenlimei, Lideluo, etc., the research on the content of algin in different parts of the kelp and the gel property thereof, Chinese food additive 2010(02): 124:. sup. + 126+142.), the content of algin in the basal part of the thallus of the kelp is between the content of algin in the middle part and the tip part of the thallus, so the content of algin in the basal part, stem (stem) or root part (root, holdfast) of the kelp cannot be ignored. However, with the current digestion and extraction technology, the liquid permeation efficiency of the thicker base, stem (stalk) or root (root, anchor) lags behind the middle and tip of the frond, and the thicker base, stem (stalk) or root (root, anchor) cannot be permeated by the reaction liquid after the digestion reaction is finished, so that the algin in the thick base cannot be extracted, and the waste of resources is caused. Therefore, improving the digestion efficiency of the base, stem (stalk) or root (root, holdfast) is of great significance to improve the yield of the traditional raw material algin.
In recent years, the above-mentioned conventional raw materials have been gradually developed into foods or foodsThe price of the feed is increased year by year, and production enterprises begin to seek other inedible brown algae as raw materials. The Lessonia (Lessonia) has obvious leaf and stem differentiation (mainly stems), the stems are compact in structure, hard in texture, difficult to digest and not suitable for eating, the content of the algin is higher than that of the traditional raw materials such as kelp and the like, the algin content can reach 40-45 g/100g, and the dense-structure Lessonia becomes a raw material for extracting the algin. The raw materials of the Thalictrum aquilegifolium on the market are dry algae bulk materials (the water content is generally 13% -18%, the raw material weight of the Thalictrum aquilegifolium or the weight average of the dry algae is calculated by the raw material of the Thalictrum aquilegifolium with the water content of 15%) imported from Chilean or Peru, and stems with the diameter of 5-20 mm and the length of 10-50 mm are taken as main materials (the stems and roots in the bulk materials are difficult to distinguish and are collectively called as the stems), and the stems generally account for more than 70% of the total weight. The literature (Zhanyan et al, proceedings of Process engineering, 2016, 16 (1): 144-one 150) adopts the existing process route of soaking-cutting-digesting, the stem of Lessonia canaliculata (one of Lessonia trabecula, Lessonia) is soaked in a 2% formaldehyde aqueous solution with 10 times of dry algae weight at 35 ℃ (soaking and synchronous color fixation) for 48h, then is crushed to 1-3 mm for digestion reaction, and Na is examined2CO3The influence of the concentration (1-2.33%), the mass ratio of the material liquid (1: 10-1: 20), the stirring speed (100-400 r/min), the digestion temperature (60-90 ℃) and the digestion time (6-10 h) on the digestion yield of the algin and the viscosity of the algin solution is optimized through an orthogonal experiment, and the determined optimal digestion condition is as follows: at a temperature of 70 ℃ and Na2CO3The concentration is 1.67%, the stirring speed is 400r/min, the mass ratio of the feed liquid is 1:15, and the digestion time is 8 h. Under the condition, the product yield of the sodium alginate is 34.80g/100g, the product viscosity is 2261.67 mPas which is much higher than 173.30 mPas of a commercial product. However, the soaking time of the Thalictrum toruloides is prolonged to 48 hours, which is about 8 times as long as that of the traditional raw materials (3-6 hours); even if the Leptospira japonica soaked for 48 hours is crushed to 1-3 mm, the yield of the algin can reach more than 30g/100g after being digested for 8 hours, and the digestion time is increased by at least 2 hours compared with the digestion time (about 3-6 hours) of the traditional raw material. The traditional digestion and extraction process is used for digesting and extracting the algin from the thunberg pine algae mainly taking stems, the soaking time and the digestion time are both greatly prolonged, and the production efficiency is severely restricted. Inventor(s):it was found that the stems of the thunberg algae were soaked at 35 deg.C, and the thunberg algae were not soaked even if the soaking time was extended to 48 hours (FIG. 4). Therefore, the Leptospira used for digestion in the literature (Zhang Yan et al, proceedings of Process engineering, 2016, 16 (1): 144-.
In conclusion, by adopting the existing algin digestion and extraction technology, for the traditional algin raw materials such as kelp and the like, the soaking efficiency and the digestion efficiency of thicker base parts, thick stems (stalks) or roots are far lagged behind those of leaves or thin stems, so that most algin in the raw materials cannot be converted and extracted, and the waste of resources is caused; for the thunberg algae mainly comprising stems with compact structures, the soaking efficiency and the digestion efficiency are further reduced, the soaking time and the digestion time are far longer than those of the traditional brown algae raw materials such as kelp, and the production efficiency is seriously influenced.
Disclosure of Invention
The invention provides a method for digesting rhizomes of brown algae to extract algin, aiming at the problems of soaking impermeability and low digestion efficiency caused by compact structure of stems (stalks) or roots (roots and fixers) in the process of digesting and extracting algin by taking brown algae as a raw material, wherein the rhizomes (raw material) comprise the base parts, stems (stalks) or roots (roots and fixers) of the brown algae or the brown algae mainly comprising the stems and the roots.
The method for extracting the algin by digesting the root and the stalk of the brown algae adds the step of rolling the root and the stalk of the brown algae before the soaking step in the existing production process route, and rolls the base part, the stalk or the root of the brown algae until cracks appear but the root is not broken. Specifically, the compression is carried out until the compression ratio is 1.2-10 or the pressure intensity is 20-350 MPa. Wherein, the compression ratio is the ratio of the diameter before rolling to the diameter after rolling in the compression direction, and the pressure is the pressure of the unit stress area of the algae block.
The invention rolls the base, the stem or the root of the brown algae until the crack appears, the water can quickly enter the crack, and then continuously permeates into the raw material from the crack, which is equivalent to shortening the actual permeation distance of the water or the reaction liquid, so that the soaking efficiency of the base, the stem (handle) or the root of the dry brown algae is improved, and the soaking time is greatly shortened; the raw materials are fully soaked to form good and sufficient water distribution inside, a good water environment is provided for the conversion reaction of the algin in the digestion step and the dissolution and diffusion of a reaction reagent and a target product, the digestion efficiency of the base part, stem (handle) or root of the brown algae is obviously improved, and the digestion time is shortened.
The specific embodiment of the invention is as follows:
the method for extracting the algin by digesting the rhizomes of the brown algae comprises the following steps:
1) rolling: rolling the base, stem and/or root of the brown algae to a compression ratio of 1.2-10;
2) soaking: adding water to submerge the rolled brown algae, and soaking for 2-8 h;
3) digestion: performing alkaline digestion on the soaked brown algae to obtain a digestive juice;
4) obtaining a product: treating the digestive juice to obtain algin.
According to the method, the water adding amount in the step 2) is 7-15 times of the weight of the brown algae (the weight of the dry algae with the water content of 15% is converted by the weight of the dry algae, and the soaking temperature is 20-35 ℃. In the alkaline digestion in the step 3), the amount of water is 10-30 times of the weight of the brown algae, and the amount of sodium carbonate is 15-40% of the weight of the brown algae.
According to the method, in the alkaline digestion in the step 3), the digestion temperature is 60-85 ℃ and the digestion time is 3-6 hours.
According to the method of the invention, in the step 3) "digestion", soda ash can be added in a solid form or Na can be added2CO3Adding the aqueous solution in a one-time manner, or adding the aqueous solution in a flow manner or a sectional adding manner; the water can be added at one time or added in a flow adding or sectional adding mode.
According to the method, the subsequent treatment of the obtained digestive juice can refer to the prior process to produce corresponding alginate products, such as slag-liquid separation according to the prior process to obtain clear liquid, calcium alginate is separated out from the clear liquid by a calcium precipitation method, alginic acid is obtained by decalcification with hydrochloric acid, target alginate is obtained by neutralization and conversion, and the like to produce corresponding alginate, and corresponding subsequent process improvement and design can also be carried out according to the actual needs and requirements of production.
The method according to the invention, wherein the rolling method in step 1) comprises one or more of rolling, pressing, squeezing and rolling, and preferably adopts a rolling device such as a roller press, a double-roller crusher and a multi-roller crusher.
According to the method, preferably, the pressing and rolling in the step 1) enables the algae blocks to be under the action of pressure intensity of 20-350 MPa, and the required compression ratio is 1.2-10.0.
The method according to the present invention, wherein the brown algae includes, but is not limited to, one or more of algae of the genera Laminaria (Laminaria), Sargassum (Sargassum), Ascophyllum (Ascophyllum), Macrocystis (Macrocystis), Ecklonia (Ecklonia), Hemiales (Tinocladia) and Lessonia. One or more of Laminaria japonica (Laminaria japonica) of Laminaria (Laminaria), Sargassum (Sargassum pallidum) of Sargassum (Sargassum), Ascophyllum nodosum (Ascophyllum nodosum) of Ascophyllum, Macrocystis grandis (Macrocystis pyrifera) of Macrocystis, Ecklonia kumia (Ecklonia maxima) of Ecklonia, Helicotina algae (Tenellaria bassiana) of Helicotina, and Thalictrum spirales (Lessonia trabecula) of Leptospira are preferable.
The method according to the present invention, wherein a washing or impurity removing step may be added before or after the rolling in step 1) according to the impurity content of the raw material.
The method according to the present invention, wherein a sorting step may be added to separate the roots and/or stems from the leaves before the rolling in step 1). Specifically, a sorting step may be added before the rolling in step 1) to separate the roots, stems and leaves, or to increase the content of the roots, stems in the raw material in step 1), according to the content of the roots, stems in the raw material. The sorting step precedes the washing or stripping step.
According to the method of the present invention, as a preferred aspect of the present invention, the rolling in step 1) may be performed by classifying the raw materials according to their diameters and then performing the rolling respectively until the compression ratio is about 1.5 to 3.3, and dividing the raw materials into three classes according to the diameter of more than 5mm but not more than 10mm, the diameter of more than 10mm but not more than 20mm, and the diameter of more than 20 mm.
According to the method, as a preferable aspect of the invention, the rolling in the step 1) can be performed until the water content of the brown algae raw material is 13% -20%, and then the brown algae raw material is rolled until the compression ratio is 1.7-2.5, and preferably, the pressure is 70-160 MPa to achieve the required compression ratio.
According to the method, as an improvement of the invention, a color fixing step can be added before the step 3) "digestion" to reduce the dissolution of impurities such as pigments in the digestion process and improve the color of the product, and the conditions of the color fixing step can refer to the color fixing conditions of the existing process. Specifically, a separate fixation step may be added before the step 2) "soaking", or fixation may be performed simultaneously during the step 2) "soaking", or a separate fixation step may be added between the step 2) "soaking" and the step 3) "digestion". The amount of the color fixing agent is 5-15% of the weight of the brown algae, and most preferably 5-15% of the weight of the dry algae. The fixing agent can use various fixing agents known in the art, such as formaldehyde, glutaraldehyde and the like, and the invention is not limited.
According to the method, 1-10% of cross-linking agents such as formaldehyde or glutaraldehyde and the like in the dry algae weight can be selectively added in the digestion process in the step 3), so that the viscosity of the algin product is further improved.
The method according to the present invention, wherein the digestion in step (3) may be performed by a combination of "simmer-churn" digestion method or "simmer-churn" digestion method with "refiner" digestion (for example, a combination of "simmer-churn" digestion with "refiner" digestion disclosed in patent CN101585890B, which is performed by a combination of "simmer-churn" digestion with "refiner-churn" digestion with "simmer-churn digestion" digestion with "refiner" digestion), or a combination of continuous stirring or continuous stirring digestion with "refiner". Preferably, a continuous stirred digestion process is used.
According to the method of the present invention, as a modification of the present invention, a step of "wet algae crushing" may be added after the step of "soaking" of step 2. The "wet algae comminution" step may be before or after a separate addition of a fixing step. The wet algae crushing is to crush the soaked brown algae to an average screening granularity d50Is 1.5 to 3 mm.
The invention has the technical characteristics that:
aiming at the problems that the brown algae mainly comprising stems and roots or the base parts, stems, roots and the like of the brown algae are difficult to soak thoroughly and reaction liquid is difficult to permeate in the digestion process, so that the soaking time is long, the digestion rate is slow, the algin yield is low and resources are wasted, the liquid-solid mass transfer performance of the raw materials is improved, and the soaking efficiency and the digestion efficiency are improved.
(1) The inventor researches and discovers that when the root, stem or root of brown algae is compressed to a compression ratio of 1.2-10, preferably under the action of pressure of 20-350 MPa, the root, stem or stem of brown algae can crack on the surface (figure 5) and inside (figure 6), but can not break into small pieces, and can not generate slag and dust.
(2) The invention rolls the brown algae to enable the base part, the stem (stalk) and the root part of the brown algae to have cracks, so that the water can quickly enter the cracks and then permeate into the raw material from the cracks, which is equivalent to shortening the actual permeation distance of the water or the reaction liquid, and obviously improves the soaking efficiency of the base part, the stem (stalk) or the root part of the dry brown algae (figures 7-10).
(3) The stem, the root and other parts in the brown algae are soaked thoroughly in advance, the low-efficiency water permeation process is stripped out from the digestion process, the step of cutting vegetables can be omitted, the digestion efficiency is improved, and the digestion time is shortened.
Compared with the prior art, the invention has the beneficial effects that:
by adding the step of rolling brown algae before the soaking step, the thicker base part, stem (stalk) and root (root and sessile apparatus) of the traditional raw materials (kelp, gulfweed, Ascophyllum nodosum and kelp) can reach the same soaking and digesting efficiency as the leaf part, and the yield of the algin is improved; for brown algae (such as Leipula rapae) raw materials mainly comprising stems and roots with compact structures, the soaking time is shortened to 8 hours from 48 hours, the digestion time can be shortened to 6 hours, the yield of algin products can reach 25-38 g/100g of brown algae (calculated by the weight of dry algae with 15 percent of water content, the same is carried out below), the yield can reach 60-90 percent, the soaking efficiency and the digestion efficiency equivalent to those of the traditional raw materials are achieved, and the time of soaking and digesting two working procedures can be shortened by more than 42 hours; in addition, the step of cutting the vegetable before digestion can be omitted.
On the other hand, for thunberg algae with a compact structure, the step of rolling brown algae is added, the soaking efficiency and the digestion efficiency are equivalent to those of traditional raw materials (kelp, gulfweed, Ascophyllum nodosum and kelp), the soaking time and the digestion time are consistent with those of the traditional raw materials, the soaking condition which is the same as that of the traditional raw materials can be set, and the digestion process condition which is close to that of the traditional raw materials provides convenience for production operation and management.
Drawings
FIG. 1 shows the filtrate after rough filtration of the digestion liquid of sea tangle.
FIG. 2 shows the residue of algal lumps after rough filtration of the digestion liquid of sea tangle.
FIG. 3 shows the penetration of the reaction solution into the stalks and roots remaining after rough filtration of the digestion solution of kelp.
FIG. 4 is a view showing the water permeation of untreated Leptospira sp stems after immersion for various periods of time, which is a cut along the axial direction after immersion.
Fig. 5 is a photograph of a stem of a leishmania sp. Wherein (a) is a photograph of an untreated stem of a thunberg algae; (b) is a photograph of the stem of the Thalictrum along the radial direction; (c) is a photograph of the stem of the Thalictrum along the axial direction.
FIG. 6 is a photomicrograph of a stem section of Leptospira sp. Wherein (a): cutting untreated Leptospira sp stems; (b) the method comprises the following steps And cutting the leishmania stems with gaps inside after rolling, wherein the white gaps are cracks.
FIG. 7 shows the water penetration of the rolled stem of Leptospermum pratense (compression ratio of 2) after soaking for 6h, wherein the soaking solution is red ink solution, and the cut surface is axial and radial.
FIG. 8 shows the water penetration of the rolled stem of Leptospermum sp.sp.sp.during 6h immersion, wherein the immersion liquid is tap water and the cut surface is axial.
FIG. 9 shows the water penetration of the rolled stem of Leptospermum sp.sp.sp.during 6h soaking, wherein the soaking solution is tap water and the cut surface is a radial one.
Fig. 10 is a graph of water absorption versus time during soaking of untreated and padded rapes stems. The pressure is the pressure of the unit stress area of the algae block.
FIG. 11 shows the yield of sodium alginate product in comparative example 1 at different digestion times.
FIG. 12 shows the yield of sodium alginate product in comparative example 3 at different digestion times.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The algin is extracted by adopting the digestion process route of the technology, the raw material is Lessonia Truperalia, the diameter range of the stem of the Lessonia Truperalis is about 5-20 mm, the Lessonia Trupeifolia is produced from Chilean and is purchased from Runlin inventment co., LTD.
(1) Rolling: adjusting the gap between two rollers of a double-roller crusher to be about 5mm, pressing 1t of the Thalictrum threadinescens to a compression ratio of about 1.2-5 through the double-roller crusher, wherein the diameter range of the Thalictrum threadinescens before compression is about 5-20 mm, and the diameter range of the Thalictrum threadinescens after compression in the rolling direction is about 4-5.5 mm.
(2) Soaking: at 20 ℃ at 10m3(about 10 times the weight of the dry algae) in tap water for 2 h.
(3) Digestion: adding soaked Thalictrum aquilegifolium into a digesting pot, adding 10m3Adding 150kg (15% of dry algae weight) of sodium carbonate into hot water (10 times of dry algae weight) at 60 + -5 deg.C, digesting at 60 deg.C under heat preservation, stewing for 45 min, stirring for 15min, and digesting for 3 hr to obtain digestive juice.
The subsequent treatment of the obtained digestive juice refers to the prior art to produce sodium alginate products, and specifically comprises the following steps: adding tap water with the weight of 100 times that of dry algae into the digestive juice, diluting, starting a 6-mesh filter for rough filtration, injecting the filtrate into a floating pool to float for 3 hours, and finely filtering the floated glue solution through a 120-200-mesh screen to obtain a clear glue solution; after the pH value of the clear glue solution is adjusted to 6.5, adding a calcium chloride solution with the mass concentration of 12% to ensure that the concentration of calcium ions in a calcification tank is between 0.045% and 0.050%, and obtaining calcium alginate through calcium precipitation; putting calcium alginate into a decalcification tank, adding water to immerse the calcium alginate, adding hydrochloric acid with the mass fraction of 31% until the pH value is 2, and decalcification for about 2 hours to obtain alginic acid; dewatering alginic acid by adopting a screw press until the water content is lower than 70%, crushing, putting the crushed alginic acid and 90% alcohol into a neutralization tank according to the proportion of 1:1, and adding a sodium hydroxide solution with the mass concentration of 40% while stirring to keep the pH value at about 8 until the pH value is unchanged; after solid-liquid separation, the sodium alginate is dried until the water content is less than 15 percent, 250kg of sodium alginate is obtained, the yield is 25.0g/100g of brown algae (by the weight of dry algae with the water content of 15 percent, the same is shown below), and the viscosity of 1 percent sodium alginate aqueous solution is 1176mPa & s.
Example 2
The process is similar to that of example 1 except that the roller spacing of the roller crusher is adjusted to 2mm, the thunberg stems are pressed to a compression ratio of 2.5-10, and finally 262kg of sodium alginate is obtained, wherein the yield is 26.2g/100g of brown algae, and the viscosity of 1% sodium alginate aqueous solution is 1165mPa · s.
Example 3
The process route of digestion process of the technology is adopted to extract algin, other than the process of the embodiment 1, a roller press is adopted, the pressure (compressive stress) applied to the lei song algae stem is about 20MPa, the lei song algae stem is pressed to the compression ratio of about 1.2, and finally, 170kg of sodium alginate is obtained, the yield is 17.0g/100g of brown algae, and the viscosity of 1% sodium alginate aqueous solution is 1345 mPa.
Example 4
The process is similar to that in example 3 except that the pressure (compressive stress) on the stem of the thunberg pine algae is 350MPa, the stem of the thunberg pine algae is pressed to a compression ratio of about 10, and 280kg of sodium alginate is finally obtained, wherein the yield is 28.0g/100g of brown algae, and the viscosity of a 1% sodium alginate aqueous solution is 1327 mPa.
Example 5
The process is similar to that of example 3 except that the pressure (compressive stress) applied to the stems of the thunberg frondosa is 200MPa, the stems of the thunberg frondosa are compressed to a compression ratio of about 2.54, and 247kg of sodium alginate is finally obtained, wherein the yield is 24.7g/100g of brown algae, and the viscosity of a 1% sodium alginate aqueous solution is 1225mPa · s.
Example 6
The process is similar to example 5 except that the soaking time is 8h, and 251kg of sodium alginate is finally obtained, the yield is 25.1g/100g of brown algae, and the viscosity of 1% sodium alginate aqueous solution is 1372mPa · s.
Example 7
The process is similar to that in example 5 except that the soaking time is 5 hr, 250kg of sodium alginate is finally obtained, the yield is 25.0g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1372mPa · s.
Example 8
The process is similar to that in example 7 except that the digestion temperature is 80 deg.C, 262kg of sodium alginate is finally obtained, the yield is 26.2g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1267mPa · s.
Example 9
The process is similar to that in example 7 except that the digestion temperature is 70 deg.C, 257kg of sodium alginate is finally obtained, the yield is 25.7g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1191mPa · s.
Example 10
Adopting the digestion process route of the technology to extract the algin, rolling the roots and the stalks of fresh kelp (Laminaria japonica) (with the water content of about 88%) to the compression ratio of 1.2 by adopting the pressure of 100MPa, and the difference of other steps is the same as the example 7, except that the consumption of the digestion water is 40 times of the dry algae weight, finally obtaining 37.4kg of sodium alginate, the yield is 26.5g/100g of brown algae, and the viscosity of the 1% sodium alginate aqueous solution is 1137 mPas.
Example 11
Adopting the digestion process route of the technology to extract the algin, airing fresh kelp (Laminaria japonica) (with the water content of about 88%) until the water content is 15%, and then taking 1t of the aired kelp to carry out rolling under the pressure of 70MPa, so that the compression ratio of the root and the stem of the kelp is about 1.7, and the other steps are the same as those of the example 7 except that the consumption of the digestion water is 40 times of the dry weight of the algae, and finally obtaining 295kg of sodium alginate, wherein the yield is 29.5g/100g of brown algae, and the viscosity of the 1% sodium alginate aqueous solution is 1137 mPa.
Example 12
Adopting the digestion process route of the technology to extract the algin, adding water into 1t of dry kelp (with the water content of 13 percent) to adjust the moisture content to 20 percent, and then adopting the pressure of 160MPa to carry out rolling, so that the compression ratio of the root and the stem of the kelp is about 2.5, the difference of other examples is the same as example 7, except that the consumption of the digestion water is 15 times of the weight of the dry kelp, 315kg of sodium alginate is finally obtained, the yield is 30.8g/100g of brown algae, and the viscosity of 1 percent of sodium alginate aqueous solution is 1221 mPa.
Example 13
Adopting the digestion process route of the technology to extract the algin, the other steps are the same as the step of the embodiment 7, except that the dosage of the sodium carbonate is 40 percent of the weight of the dry algae, 267kg of the sodium alginate is obtained, the yield is 26.7g/100g of brown algae, and the viscosity of the 1 percent sodium alginate aqueous solution is 1115 mPa.s.
Example 14
Adopting the digestion process route of the technology to extract the algin, the other steps are the same as the step of the embodiment 7, except that the dosage of the sodium carbonate is 25 percent of the weight of dry algae, 247kg of the sodium alginate is obtained, the yield is 24.7g/100g of brown algae, and the viscosity of 1 percent of sodium alginate aqueous solution is 1227mPa & s.
Example 15
The process is similar to that in example 14 except that the digestion time is 6h, 323kg of sodium alginate is obtained, the yield is 32.3g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1415mPa · s.
Example 16
The digestion process route adopted by the technology is adopted to extract algin, and the other steps are the same as the example 15, except that the rapana is classified according to the diameter, and then is rolled by a roller crusher, the diameter is larger than 5mm but smaller than or equal to 10mm, the distance between rollers is 3mm, the distance between rollers is larger than 10mm but smaller than or equal to 20mm is 6mm, the distance between rollers is larger than 20mm and is 11mm, the three steps are divided into three steps, the three steps are respectively rolled until the compression ratio is about 1.5-3.3, sodium alginate 321kg is obtained, the yield is 32.1g/100g of brown algae, and the viscosity of 1% sodium alginate aqueous solution is 1371 mPa.
Example 17
Adopting the digestion process route of the technology to extract the algin, the other steps are the same as the example 15, except that the raw material Leipara is sprayed with water and is subjected to moisture regulation to form that the water content is 20%, the diameter is more than 5mm but less than or equal to 10mm, the adopted roller spacing is 3mm, the adopted roller spacing is 6mm, the adopted roller spacing is 11mm, the diameter is more than 20mm, the three steps are divided into three grades, the three grades are respectively rolled until the compression ratio is about 1.5-3.3, sodium alginate 321kg is obtained, the yield is 32.1g/100g of brown algae, and the viscosity of 1% sodium alginate aqueous solution is 1379 mPa.
Example 18
The process is similar to that in example 15 except that the digestion process is carried out for 45 min and 15min, and the digestion is carried out for 6h to obtain 330kg of sodium alginate, the yield is 33.0g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1357mPa · s.
Example 19
The process is similar to that in example 15 except that formaldehyde in 10% dry weight is added into soaking water at the beginning of soaking to obtain 331kg sodium alginate in yield of 33.1g/100g and sodium alginate solution in 1% concentration of 2217mPa · s in viscosity and yellowish color after digesting for 6 hr.
Example 20
The process is similar to that in example 15 except that formaldehyde in 5% dry weight is added into the digesting pot for 6 hr to obtain 333kg sodium alginate in 33.3g/100g yield and 1% concentration water solution of sodium alginate in 2615mPa · s viscosity.
Example 21
The process for extracting algin by digestion route of the technology is the same as example 15 except that brown algae is crushed to d after soaking50384kg of sodium alginate was obtained at 2mm, yield 38.4g/100g brown algae, viscosity of 1% sodium alginate solution was 1335mPa · s.
Example 22
The process is similar to that in example 20 except that 10% formaldehyde is added to soaking water to obtain 376kg sodium alginate after 6 hr digestion, and has yield of 37.6g/100g sodium alginate, viscosity of 1% sodium alginate solution of 2317mPa · s, light yellow color and pH 7.05.
Comparative example 1
Extracting algin by digestion process route of soaking-pulverizing-digesting, the raw material is the same as example 1, soaking Thalictrum toruloides in tap water 10 times of the weight of dry algae at 20 deg.C for 8h, pulverizing to powder d50Digesting 6.5mm (the particle size is 3-10 mm), digesting and processing conditions are the same as example 13, after digesting for a certain time, processing the digestion solution to obtain sodium alginate, performing subsequent processing on the digestion solution is the same as example 1, the yield of the sodium alginate product obtained under different digestion times is shown in figure 11, when the digestion time reaches 10h, the yield of the sodium alginate product is 15.0g/100g brown algae, and the viscosity of a 1% sodium alginate aqueous solution is 365mPa · s.
Comparative example 2
Adopts the digestion process route of soaking-crushing-digestion to extract the algin, and the other steps are the same as the comparative example 1, except that the serratia marcescens which are soaked in tap water with 10 times of the weight of dry algae for 8 hours at the temperature of 20 ℃ are crushed into d50Digesting the brown algae for 8 hours when the grain size is 2mm (the grain size is 1-3 mm), wherein the yield of the sodium alginate digested for 8 hours is 25.0g/100g of brown algae, and the viscosity of a 1% sodium alginate aqueous solution is 710 mPas.
Comparative example 3
Adopts a digestion process route of soaking-crushing-digestion to extract algin, and the other steps are the same as the comparative example 1, except that the larch spirulina is soaked in a 2 percent formaldehyde aqueous solution with 10 times of the weight of dry algae (soaking and synchronous color fixation) for 48 hours at 35 ℃, and then crushed to d50Digesting 2mm (particle size range 1-3 mm), after digesting for a certain time, processing the digestion solution to obtain sodium alginate, wherein the yield of sodium alginate products under different digestion time is shown in figure 12. The yield of the sodium alginate product obtained by digesting for 8 hours is 34.4g/100g of brown algae, the viscosity of 1 percent sodium alginate aqueous solution is 2160 mPa.s, but the soaking time and the digesting time are both obviously longer than those of the traditional raw materials, and the existing production program can not be adopted for production.
The present invention may be embodied in many different forms and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (15)
1. A method for extracting algin by digesting rhizomes of brown algae bases comprises the following steps:
1) rolling: rolling the base, stem and/or root of dry brown algae by adopting the pressure of 20-350 MPa to a compression ratio of 1.2-10 so that the dry brown algae has cracks and is not broken into small blocks, wherein the compression ratio is the ratio of the diameter before rolling in the compression direction to the diameter after rolling;
2) soaking: adding water to submerge the rolled brown algae, and soaking for 2-8 h;
3) digestion: performing alkaline digestion on the soaked brown algae to obtain a digestive juice;
4) obtaining a product: treating the digestive juice to obtain algin.
2. The method as claimed in claim 1, wherein the water addition amount in the step 2) is 7-15 times of the weight of the brown algae, and the soaking temperature is 20-35 ℃; wherein the brown algae weight is calculated by converting the brown algae into dry algae with water content of 15%.
3. The method as claimed in claim 1, wherein in the alkaline digestion in the step 3), the amount of water is 10-30 times of the weight of the brown algae, and the amount of sodium carbonate is 15-40% of the weight of the brown algae; wherein the brown algae weight is calculated by converting the brown algae into dry algae with water content of 15%.
4. The method according to claim 3, wherein in the alkaline digestion in the step 3), the digestion temperature is 60-85 ℃ and the digestion time is 3-6 h.
5. The method according to claim 1, wherein in the alkaline digestion in the step 3), the digestion temperature is 60-85 ℃ and the digestion time is 3-6 h.
6. The method according to any one of claims 1 to 5, wherein the rolling method of step 1) comprises one or more of rolling, pressing and extruding.
7. The method according to any one of claims 1 to 5, wherein a washing or impurity removal step is added before or after the rolling in step 1).
8. The method according to any one of claims 1 to 5, wherein a sorting step is added to separate the roots and/or stems from the leaves prior to said rolling in step 1).
9. The method according to any one of claims 1 to 5, wherein the step 1) comprises the steps of classifying the root, stem and/or root of the brown algae according to the diameter and then respectively rolling the classified root, stem and/or root to a compression ratio of 1.5-3.3; wherein, the rolling is respectively carried out according to three grades with the diameter of more than 5mm but less than or equal to 10mm, the diameter of more than 10mm but less than or equal to 20mm and the diameter of more than 20 mm.
10. The method as claimed in any one of claims 1 to 5, wherein the brown algae is treated to have a water content of 13% to 20% in step 1), and then is rolled to a compression ratio of 1.7 to 2.5.
11. The method as claimed in claim 10, wherein the step 1) is carried out by rolling at a pressure of 70 to 160 MPa.
12. The method according to any one of claims 1 to 5, wherein the fixing is carried out by adding a fixing agent before the soaking in step 2), or during the soaking in step 2), or after the soaking in step 2) and before the digestion in step 3).
13. The method according to any one of claims 1 to 5, wherein 1% to 10% by dry algal weight of formaldehyde or glutaraldehyde is added during the digestion in step 3).
14. A method according to any one of claims 1-5, characterized in that digestion in step 3) is carried out by a combination of agitation and refining, or by a continuous agitation digestion, or by a combination of continuous agitation and refining.
15. The method according to any one of claims 1 to 5, wherein a wet algae comminution step is added after the soaking in step 2).
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| CN101906174A (en) * | 2010-07-29 | 2010-12-08 | 中国水产科学研究院黄海水产研究所 | Improved method of fresh kelp high-efficiency pretreatment and algin extraction processes for chemical engineering |
| CN103360509A (en) * | 2013-07-16 | 2013-10-23 | 山东洁晶集团股份有限公司 | Method for preparing alginic acid and alginate by taking fresh sargassum as raw material |
| CN104448031A (en) * | 2013-09-12 | 2015-03-25 | 山东洁晶集团股份有限公司 | Improved method of traditional sodium alginate production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101906174A (en) * | 2010-07-29 | 2010-12-08 | 中国水产科学研究院黄海水产研究所 | Improved method of fresh kelp high-efficiency pretreatment and algin extraction processes for chemical engineering |
| CN103360509A (en) * | 2013-07-16 | 2013-10-23 | 山东洁晶集团股份有限公司 | Method for preparing alginic acid and alginate by taking fresh sargassum as raw material |
| CN104448031A (en) * | 2013-09-12 | 2015-03-25 | 山东洁晶集团股份有限公司 | Improved method of traditional sodium alginate production process |
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