CN108329400B - Method for extracting algin from digestion Leptospira sp - Google Patents
Method for extracting algin from digestion Leptospira sp Download PDFInfo
- Publication number
- CN108329400B CN108329400B CN201710042249.2A CN201710042249A CN108329400B CN 108329400 B CN108329400 B CN 108329400B CN 201710042249 A CN201710042249 A CN 201710042249A CN 108329400 B CN108329400 B CN 108329400B
- Authority
- CN
- China
- Prior art keywords
- digestion
- soaking
- algae
- algin
- thunberg
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- C08B37/006—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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention belongs to the technical field of seaweed chemical industry, and particularly relates to a method for extracting algin from Leptospira sp. The method for extracting algin by digesting the thunberg pine algae comprises the following steps: 1) crushing: pulverizing Rapana Thomasiana to average sieving particle size d50Not more than 5 mm; 2) soaking: adding water to submerge the crushed thunberg algae, and soaking for 2-8 h; 3) digestion: carrying out alkaline digestion on the soaked thunberg sponge to obtain a digestive juice; 4) obtaining a product: treating the digestive juice to obtain algin. The invention improves the soaking efficiency of the raw materials, so that the raw materials can be soaked thoroughly in a short time; the raw materials are fully soaked to form good and sufficient water distribution inside, so that a good water environment is provided for full progress of alginate conversion reaction in a digestion step and dissolution and diffusion of a reaction reagent and a target product, the digestion efficiency is improved accordingly, and the digestion time is shortened.
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 Leptospira sp as a raw material.
Background
Algin is a generic name for alginic acid and its salts, a plant polysaccharide found in brown algae. The algin has good thickening property, emulsifying property, film forming property, stability and the like, and is widely applied to the industries of food, medicine, textile, wastewater treatment, daily chemicals and the like. Algin generally refers to sodium alginate in the market, and the quality specification of the algin is mainly divided according to the viscosity of 1% (mass percentage concentration, the same below) sodium alginate aqueous solution, for example, the national standard (GB 1976-2008) of algin for food additives is divided into three specifications of high, medium and low according to the viscosity range of 1% sodium alginate aqueous solution, low-viscosity algin is below 150 mPa.s, medium-viscosity algin is between 150 and 400 mPa.s, and the viscosity of high-viscosity algin needs to be higher than 400 mPa.s. Because the high-viscosity adhesive has better thickening stability and has wider application requirements in the fields of food, daily chemicals, printing and dyeing and the like, the main product of a general production enterprise is the high-viscosity adhesive with the viscosity of more than 400mPa & s.
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 through 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 algin production process, and the digestion effect directly influences the yield and the viscosity of the product.
Because the raw material of industrial brown algae is mainly dry algae, in the traditional technology for digesting and extracting algin from brown algae, soaking and cutting vegetables are generally taken as pretreatment steps of a digestion step, and soaking, cutting vegetables and digestion in the existing production process are divided into three procedures of a 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%, the product viscosity of the sodium alginate (referring to 1% sodium alginate aqueous solution) is generally 400-700 mPa.s, and the requirement of high-viscosity glue can be met.
With the large amount of raw materials of brown algae purchased by algin manufacturing enterprises and the raw materials of brown algae with loose structure being developed into food or high-grade feed, the price of raw materials of brown algae is rising year by year, and the raw materials of brown algae which are not suitable for eating are gradually becoming the raw materials for producing algin. 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 algin is higher than that of kelp and other raw materials and can reach 45g/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 the root base parts in the bulk materials are difficult to distinguish and are collectively called as the stems), and generally account for more than 70% of the total weight. The literature (Zhanyan et al, proceedings of Process engineering, 2016, 16 (1): 144-150) adopts the current process route of 'soaking-cutting-digesting', the stem of Lessonia frabica (one of Lessonia trabecula, Lessonia) is soaked (soaked for synchronous fixation) in 2% formaldehyde aqueous solution 10 times of the weight of dry algae at 35 ℃ for 48h, and then is pulverized to 1 @ fDigestion reaction was carried out at 3mm, and Na was 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 orthogonal experiments, and infrared spectrum qualitative analysis is carried out on the algin. The results show that the optimal digestion conditions are: 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 time is 8 h. Under the condition, the yield of the sodium alginate product is 34.80g/100g, the viscosity of the product is 2261.67 mPas which is much higher than 173.30 mPas of the commercial product. However, the soaking time of the Thalictrum toruloides needs 48 hours, which is about 8 times as long as that of the traditional raw materials (3-6 hours); even if the Thalictrum threadeduncum soaked for 48 hours is crushed to 1-3 mm, the digestion time (about 3-6 hours) is increased by at least 2 hours compared with the digestion time of the traditional raw materials, and the production efficiency is severely restricted.
In summary, if the prior process route of soaking, cutting and digesting is adopted to extract the algin from the thunberg pine algae, the production efficiency is far behind that of the traditional raw materials, and the industrial technology for digesting and extracting the algin from the thunberg pine algae is needed to be provided.
Disclosure of Invention
The invention provides a method for digesting and extracting algin by taking Leptospermum roseum as a raw material, aiming at the problems of long soaking time, incomplete soaking of Leptospermum roseum stems and root bases and long digesting time caused by the incomplete soaking in the process flow for digesting and extracting the algin by taking the Leptospermum roseum as the raw material.
The method for extracting algin by digesting the thunberg pine algae changes the traditional process route of 'soaking-cutting vegetables-digesting' into the method that the dry thunberg pine algae is crushed to the average screening granularity d before soaking50(the grain size corresponding to the cumulative grain size distribution mass percentage of 50%) is not more than 5mm, and then the process route of 'crushing-soaking-digesting' of soaking and digesting is carried out (figure 1).
The invention changes the traditional process route of 'soaking, cutting vegetable and digesting' into the method that the dry thunberg larch algae is crushed to the average screening granularity d before soaking50After the process route of crushing, soaking and digesting is carried out after the thickness is not more than 5mm, the soaking efficiency of the raw materials is improved, so that the raw materials can be soaked thoroughly in a short time; the raw materials are fully soaked to form good and sufficient water distribution inside, so that a good water environment is provided for full progress of alginate conversion reaction in a digestion step and dissolution and diffusion of a reaction reagent and a target product, the digestion efficiency is improved accordingly, and the digestion time is shortened.
The specific embodiment of the invention is as follows:
the method for extracting algin by digesting the thunberg pine algae comprises the following steps:
1) crushing: pulverizing Rapana Thomasiana to average sieving particle size d50Not more than 5 mm;
2) soaking: adding water to submerge the crushed thunberg algae, and soaking for 2-8 h;
3) digestion: carrying out alkaline digestion on the soaked thunberg sponge 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 preferably 7-15 times of the weight of the thunberg sponge (calculated as the weight of dry algae with the water content of 15 percent, the same below), and the soaking temperature is 20-35 ℃.
According to the method of the invention, preferably, in the alkaline digestion in the step 3), the amount of water is 10-30 times of the weight of the thunberg sponge (calculated by the weight of dry algae with water content of 15%), and the amount of sodium carbonate is 15-40% of the weight of the thunberg sponge. Further preferably, 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 digestion in the step 3), sodium carbonate can be added in a solid form or in an aqueous solution form; the additive can be added at one time, or fed-batch or segmented supplement mode can be adopted; the water can be added at one time or added in a flow adding or sectional adding mode.
According to the process of the invention, step 1) the average sieve size d50More preferably 3.2 to 4 mm.
The method according to the present invention, wherein a washing or impurity removing step may be added before or after the pulverization in step 1).
According to the method, a color fixing agent can be added for color fixing before the soaking in the step 2), or in the soaking process in the step 2), or after the soaking in the step 2) and before the digestion in the step 3), so that the dissolution of impurities such as pigments in the digestion process is reduced, the color of the product is improved, and the conditions of the color fixing step can refer to the color fixing conditions of the existing process; further preferably, the amount of the color fixing agent is 5-15% of the weight of the thunberg.
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 Thalictrum rapae to an average screening granularity d50Not more than 3 mm.
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 added in the process of the step 3 'digestion', so that the viscosity of the algin product is further improved.
The method of the invention, wherein the digestion in the step 3) can adopt a soaking and stirring combined leaching method or a continuous stirring leaching method. Preferably, a continuous stirred digestion process is used.
According to the method of the invention, the subsequent treatment of the digestive juice obtained in the step 4) can refer to the existing process to produce corresponding alginate products, such as obtaining clear liquor by performing residue-liquid separation according to the existing process, separating calcium alginate from the clear liquor by a calcium precipitation method, obtaining alginic acid by decalcification with hydrochloric acid, obtaining target alginate by neutralization and conversion and the like to produce corresponding alginate, and corresponding subsequent process improvement and design can also be performed according to the actual needs and requirements of production.
The technical scheme provided by the invention is as follows:
in the literature (Zhangyan and the like, proceedings of process engineering, 2016, 16 (1): 144-150), the algin is digested and extracted by taking Leptospermum pratense as a raw material by adopting an industrially existing 'soaking-vegetable cutting-digesting' process, the soaking time of the Leptospermum pratense is prolonged to 48 hours from 3-6 hours of the traditional raw material (kelp, gulfweed and the like), and the Leptospermum pratense soaked for 48 hours is crushed into 1-3 mm and then used for digestion. Even under the optimal digestion conditions of the thunberg thunbergii given by the literature, the digestion efficiency of the thunberg thunbergii is still remarkably laggard behind that of the traditional raw materials, the yield of the algin equivalent to that of the traditional raw materials is achieved, the digestion time is still 8 hours, and the digestion time is far longer than that of the traditional raw materials (about 3-6 hours).
The inventor soaks the unbroken thunberg stems at 35 ℃, cuts the thunberg stems soaked for different time (figure 2), and finds that the water penetration thickness is only about 2-3 mm, wherein the thunberg stems soaked for 48h are not soaked. The inventor further crushed the dried thunberg algae to different particle sizes and then soaked, and the change of the water absorption rate at 20 ℃ along with the soaking time is shown in figure 3. As can be seen from FIG. 3, the water absorption increases with decreasing particle size at the same soaking time, particularly when the average sieve particle size is from d50Decrease to d 6mm50When the grain size is 5mm, the amplification is maximum, the grain size continues to be reduced, and the increase of the water absorption rate is no longer obvious; under the same granularity, the water absorption rate increases with the prolonging of the soaking time, but the increase gradually decreases, and the water absorption basically stops after the soaking time reaches a certain water absorption rate. Average sieve particle size d50When the diameter is 5mm, the water absorption of the thunberg stems can reach more than 210% when the thunberg stems are soaked for 2.5 hours, the water absorption is basically stopped when the thunberg stems are soaked for 6 hours, and the water absorption can reach 240%. However, when the average sieve particle size d50When the thickness is 6mm, the water absorption can reach 210 percent (figure 3) after soaking for more than 6 hours, and the water absorption reaches 220 percent after 18 hours, so that the water absorption is basically stopped. Cutting off the Thalictrum amansii soaked for different time, and finding out the average screening particle size d50When the diameter is 5mm, the stem of the ralstonia thunbergii is basically soaked thoroughly when the ralstonia thunbergii is soaked for 2.5h (figure 4); when the average sieve size d50When the thickness is 6mm, the water is continuously soaked for 36h after 18h of water absorption stagnation, and the penetration thickness of the water in the soaked rapana is only about 2-3 mm (figure 5). It can be seen that the literature (Zhang Yan, etc.)Proceedings of engineering, 2016, 16 (1): 144-150) the riparian algae used for digestion is the riparian algae, and the digestion process is actually to digest and soak the riparian algae at the same time, so even if the riparian algae soaked for 48 hours is crushed to 1-3 mm for digestion, the digestion time is still 8 hours under the optimal digestion condition, which is much longer than that of the traditional raw materials.
The inventors have thus found that there is a certain limit or saturation of water penetration in the stem of the thunberg algae, which is the source of the thunberg algae that cannot be soaked through after a long soaking time, much longer than the usual soaking time, whereas the impermeability of the thunberg algae is the source of the long digestion time. When the algin is digested and extracted by taking the thunberg as a raw material, the algin is difficult to be soaked thoroughly by prolonging the soaking time, the digesting time is difficult to be shortened by simply adjusting the process conditions of the traditional process, the traditional digesting process of the brown algae with loose structures such as kelp or gulfweed cannot be simply used, and the process route needs to be changed.
Therefore, the inventor proposes a process route which changes the traditional process route of 'soaking-vegetable cutting-digestion' into a process route of 'crushing-soaking-digestion'. Because the effective penetration distance of water in the soaked Thalictrum aquilegifolium stems is only about 2-3 mm, the soaked Thalictrum aquilegifolium expands to about 1.3-1.5 times of the particle size of dry algae, and the Thalictrum aquilegifolium stems are soaked efficiently by combining the water absorption (figure 3) and water penetration (figures 4 and 5) of the Thalictrum aquilegifolium in the soaking process with the change of the particle size, so as to crush the Thalictrum aquilegifolium stems to the average screening particle size d50Preferably less than or equal to 5 mm. By pulverizing dried Rapana to average sieve particle size d50Not more than 5mm, so that the thunberg pine algae are soaked thoroughly in the soaking step; furthermore, by stripping the inefficient moisture penetration process from digestion, digestion efficiency is improved and digestion time is shortened. Thus, the production efficiency is improved by shortening the soaking and digestion time.
Compared with the prior art, the invention has the beneficial effects that:
the traditional process route of 'soaking, vegetable cutting and digesting' is changed into that the dried thunberg larch algae is crushed to the average screening granularity d before soaking50A 'crushing-soaking-digesting' process route of soaking and digesting after the diameter is not more than 5mm, and the soaking time is determined by the traditional techniqueThe 48 hours of the process treatment of the Thymelaeaceae rapana is shortened to 8 hours, so that the Thymelaeaceae rapana can be basically soaked thoroughly, the digestion time can be shortened to 3-6 hours, the yield of the algin product can reach 25g/100 g-38 g/100g of brown algae (calculated as the weight of dry algae with the water content of 15 percent, the same below), and the yield can reach 60-90 percent.
By improving the soaking efficiency and the digestion efficiency, the time of the soaking procedure and the digestion procedure can be shortened by more than 42 hours, the production period is greatly shortened, and the production benefit is improved.
Drawings
FIG. 1 is a process scheme of the method for extracting algin by digesting Leptospira sp.
FIG. 2 shows the water penetration thickness of unpulverized stems of Leptospira sp.
Fig. 3 is a graph showing the water absorption rate of the thunberg stems crushed to different particle sizes as a function of the soaking time.
FIG. 4 shows the water penetration of the stems of the thunberg algae crushed to different particle sizes after being soaked for 2.5 h.
FIG. 5 is the average sieve particle size d50Liquid permeation condition of 6mm thunberg stems after soaking for 36 h.
FIG. 6 shows the yield of sodium alginate product obtained by the process of the present invention at different digestion times (example 14).
FIG. 7 shows the yield of sodium alginate product obtained by digesting Leptospira sp with the prior art 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, and the raw material is Lessonia Trascula which is produced from Chilean and purchased from Runlin inventment co., LTD.
(1) Crushing: pulverizing 1t Leptospira japonica into average sieving granularity d by a pulverizer50＝5mm。
(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, and 260kg of sodium alginate is obtained, the yield is 26.0g/100g brown algae (calculated by the weight of dry algae with the water content of 15 percent, the same is used below), and the viscosity of 1 percent sodium alginate aqueous solution is 1795 mPas.
Example 2
The process route of the digestion process adopted to extract the algin is the same as that of the process route of the embodiment 1 except that the soaking time is 4.5 hours, 266kg of sodium alginate is finally obtained, the yield is 26.6g/100g of brown algae, and the viscosity of 1 percent sodium alginate aqueous solution is 1763 mPa.s.
Example 3
The process is the same as example 1 except that soaking time is 8h, 270kg of sodium alginate is finally obtained, yield is 27.0g/100g brown algae, and viscosity of 1% sodium alginate solution is 1651mPa · s.
Example 4
The process is similar to that of example 3 except that the digestion temperature is 80 deg.C, 292kg of sodium alginate is finally obtained, the yield is 29.2g/100g brown algae, and the viscosity of 1% sodium alginate solution is 1265mPa · s.
Example 5
The process is similar to that of example 3 except that the digestion temperature is 70 deg.C, 281kg sodium alginate is obtained, the yield is 28.1g/100g brown algae, and the viscosity of 1% sodium alginate solution is 1479mPa · s.
Example 6
The process route of the digestion process adopted to extract the algin is the same as that of the example 5 except that the consumption of the digestion water is 40 times of the dry algae weight, and 287kg of sodium alginate is finally obtained, the yield is 28.7g/100g of brown algae, and the viscosity of the 1% sodium alginate aqueous solution is 1537mPa & s.
Example 7
The process is similar to example 5 except that 15 times of the dry weight of the digestion water is used to obtain 285kg of sodium alginate, the yield is 28.5g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1521mPa · s.
Example 8
The process route of digestion of the technology is adopted to extract algin, and the other steps are the same as example 7 except that the dried thunberg is crushed to the average screening granularity d50292kg of sodium alginate was obtained at 4mm, yield 29.2g/100g brown algae, and viscosity of 1% sodium alginate aqueous solution was 1615 mPas.
Example 9
The process route of digestion of the technology is adopted to extract algin, and the other steps are the same as example 7 except that the dried thunberg is crushed to the average screening granularity d50301kg of sodium alginate was obtained at 3.2mm, yield 30.1g/100g brown algae, viscosity of 1% sodium alginate aqueous solution was 1815mPa · s.
Example 10
The process is similar to example 9 except that sodium carbonate is 40 wt% of dry algae to obtain 318kg sodium alginate, and the yield is 31.8g/100g brown algae, and the viscosity of 1% sodium alginate solution is 1015 mPa.s.
Example 11
The process is similar to example 9 except that sodium carbonate is 25 wt% of dry algae to obtain sodium alginate 310kg, yield is 31.0g/100g brown algae, and viscosity of 1% sodium alginate solution is 1720mPa · s.
Example 12
The process is similar to that of example 11 except that the digestion time is 4 hr to obtain 327kg sodium alginate in the yield of 32.7g/100g brown algae and the viscosity of 1% concentration water solution of sodium alginate is 1519mPa · s
Example 13
The process is similar to that of example 11 except that the digestion time is 6 hr to obtain 368kg sodium alginate in 36.8g/100g brown algae, and the viscosity of 1% sodium alginate solution is 1650mPa · s.
Example 14
The process is similar to that in example 11, except that formaldehyde with 10% dry algae weight is added into soaking water at the beginning of soaking, 306kg sodium alginate is obtained after 3h digestion, 335kg sodium alginate is obtained after 4h digestion, 365kg sodium alginate is obtained after 6h digestion time is prolonged, the yield is 36.5g/100g brown algae, the viscosity of 1% sodium alginate aqueous solution is 2352mPa · s, the color is light yellow, the pH value is 7.05, the yield of sodium alginate in different digestion time is shown in FIG. 6, and the yield of sodium alginate in the process is higher than that in the prior art (FIG. 7) by 4-7 g/100g in the same digestion time.
Example 15
The process is similar to that in example 13 except that the digestion mode is changed from braising for 45 min and stirring for 15min to continuously stirring, and the digestion is carried out for 6h to obtain 380kg of sodium alginate, the yield is 38.0g/100g of brown algae, and the viscosity of 1% sodium alginate solution is 1657 mPa.
Example 16
The process is similar to that in example 13 except that formaldehyde in 5% dry weight is added into the digesting pot at the beginning of digestion to obtain 370kg sodium alginate in 37.0g/100g yield and 2647mPa · s viscosity of 1% sodium alginate solution.
Example 17
The process for extracting algin by digestion route of the technology is otherwise the same as example 13, except that the soaked Thalictrum aquilegifolium is further pulverized to d50After digesting for 6h 2mm, 375kg of sodium alginate was obtained, the yield was 37.5g/100g brown algae, and the viscosity of 1% sodium alginate solution was 1665mPa · s.
Comparative example 1
Extracting algin by digestion process of soaking-pulverizing-digesting, soaking stem of Lessonia trabecula (one of Lessonia) in 2% formaldehyde aqueous solution 10 times of dry algae weight at 35 deg.C for 48 hr, and pulverizing to powder50Digesting 2mm (particle size range is 1-3 mm), wherein the digestion temperature is 70 ℃, the water consumption is 15 times of the weight of dry algae, the sodium carbonate consumption is 25% of the weight of the dry algae, after digesting for a certain time, the digestion solution is treated to obtain sodium alginate, the treatment on the digestion solution is the same as that in example 1, the yield of sodium alginate products under different digestion times is shown in figure 7, wherein the yield of sodium alginate digested for 3 hours is 24.7g/100g of brown algae, the yield of sodium alginate digested for 6 hours is 32.2g/100g of brown algae, and the yield of sodium alginate is about 1.3-7 g/100g lower than that of sodium alginate adopting the technology under the same digestion time; the yield of the sodium alginate of 8h is 34.4g/100g brown algae, the viscosity of 1 percent sodium alginate aqueous solution is 2160 mPa.s, but the soaking time and the digestion time are both obviously longer than those of the traditional raw materials, and the production can not be realized by adopting the current production program.
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 (10)
1. A method for extracting algin from Thalictrum japonicum comprises the following steps:
1) crushing: pulverizing Rapana to average sieving particle sized 50Not more than 5 mm;
2) soaking: adding water to submerge the crushed thunberg algae, and soaking for 2-8 h;
3) digestion: carrying out alkaline digestion on the soaked Leptospira sp to obtain a digestion solution, wherein the digestion temperature is 60-85 ℃, and the digestion time is 3-6 hours;
4) obtaining a product: treating the digestive juice to obtain algin.
2. The method according to claim 1, wherein the water addition amount in the step 2) is 7-15 times of the weight of the Thamnolia vermicularis, and the soaking temperature is 20-35 ℃, wherein the Thamnolia vermicularis is calculated by converting the Thamnolia vermicularis into dry algae with the water content of 15%.
3. The method according to claim 1, wherein in the alkaline digestion in step 3), the amount of water is 10-30 times of the weight of the Thamnolia vermicularis, and the amount of sodium carbonate is 15-40% of the weight of the Thamnolia vermicularis, wherein the weight of the Thamnolia vermicularis is calculated by converting the Thamnolia vermicularis into dry algae with a water content of 15%.
4. The method of any of claims 1-3, wherein the average sieved particle size of step 1) isd 50Is 3.2-4 mm.
5. A method according to any one of claims 1 to 3, characterized in that a washing or impurity removal step is added before or after the comminution in step 1).
6. The method according to any one of claims 1 to 3, 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).
7. The method according to claim 6, wherein the fixing agent is used in an amount of 5% to 15% by weight of the Thamnolia vermicularis, wherein the Thamnolia vermicularis is calculated by converting Thamnolia vermicularis into dry algae having a water content of 15%.
8. The method according to any one of claims 1 to 3, wherein the step of adding wet algae comminution is performed after the soaking in step 2).
9. The method according to any one of claims 1 to 3, wherein 1 to 10% by weight of the thunberg algae calculated as dried algae having a water content of 15% is added during the digestion in step 3) as formaldehyde or glutaraldehyde.
10. A method according to any one of claims 1 to 3, wherein digestion in step 3) is by a combination of gentle agitation and leaching or by a continuous agitation leaching process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710042249.2A CN108329400B (en) | 2017-01-20 | 2017-01-20 | Method for extracting algin from digestion Leptospira sp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710042249.2A CN108329400B (en) | 2017-01-20 | 2017-01-20 | Method for extracting algin from digestion Leptospira sp |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108329400A CN108329400A (en) | 2018-07-27 |
| CN108329400B true CN108329400B (en) | 2020-11-13 |
Family
ID=62921617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710042249.2A Active CN108329400B (en) | 2017-01-20 | 2017-01-20 | Method for extracting algin from digestion Leptospira sp |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108329400B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102492053A (en) * | 2011-12-28 | 2012-06-13 | 青岛明月海洋科技有限公司 | Preparation method of high-viscosity alginate |
| WO2015067971A1 (en) * | 2013-11-11 | 2015-05-14 | Marine Biopolymers Ltd | Method of processing seaweed and related products |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2283146A4 (en) * | 2008-04-29 | 2012-02-22 | Marshall University Res Corp | Methods of producing bacterial alginates |
| CN103360509B (en) * | 2013-07-16 | 2016-08-10 | 山东洁晶集团股份有限公司 | Alginic acid and the method for alginic acid salt is prepared for raw material with fresh sargassum |
| CN104448031B (en) * | 2013-09-12 | 2017-01-18 | 山东洁晶集团股份有限公司 | Improved method of traditional sodium alginate production process |
| CN105754011B (en) * | 2016-03-21 | 2018-01-30 | 青岛海之林生物科技开发有限公司 | A kind of preparation technology of water soluble algae acid |
-
2017
- 2017-01-20 CN CN201710042249.2A patent/CN108329400B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102492053A (en) * | 2011-12-28 | 2012-06-13 | 青岛明月海洋科技有限公司 | Preparation method of high-viscosity alginate |
| WO2015067971A1 (en) * | 2013-11-11 | 2015-05-14 | Marine Biopolymers Ltd | Method of processing seaweed and related products |
Non-Patent Citations (1)
| Title |
|---|
| Viscoelastic properties of ultra-high viscosity alginates;Storz Henning et al.;《RHEOLOGICA ACTA》;20091210;第49卷(第2期);第155-167页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108329400A (en) | 2018-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106939325A (en) | A kind of preparation method of ox bone collagen albumen | |
| CN102268327A (en) | Method for orange peel essential oil and pectin combined production | |
| CN104592416A (en) | High-quality natural pectin extraction technology | |
| CN105622782B (en) | A kind of enzyme process substitutes the preparation method of alkalinity extraction fragrant plant mentioned in ancient texts agar | |
| CN108329400B (en) | Method for extracting algin from digestion Leptospira sp | |
| CN106617115B (en) | Method for separating soluble dietary fiber from waste liquid of momordica grosvenori production | |
| CN105924543A (en) | Environment-friendly plant pectin preparation method | |
| CN102726599A (en) | Preparation process for novel bone meal | |
| CN104448031B (en) | Improved method of traditional sodium alginate production process | |
| JP2015183020A (en) | Powdery cellulose | |
| CN108329401B (en) | Method for extracting algin by quickly digesting brown algae | |
| CN103497261A (en) | Chondroitin sulfate production process | |
| CN108329402B (en) | Method for extracting algin by digesting brown algae rhizome | |
| CN109336997B (en) | Method for extracting inulin from jerusalem artichoke at low temperature | |
| CN108530506A (en) | A kind of Extractive Methods on Baicalin Recovery from Scutellaria baicalemsis Georgi of cold fermentation Microwave Water cycle | |
| CN107641159B (en) | Production process of low-viscosity whitening carrageenan | |
| CN106277516B (en) | The method of water reuse is adsorbed in a kind of production of stevioside | |
| CN109553698A (en) | A kind of pectin from lemon peel pre-treating method | |
| CN103803689A (en) | Low-molecular-weight pectin composite flocculant and online extraction process thereof | |
| DE439540C (en) | Process for processing and digesting materials containing alumina | |
| CN108651918A (en) | A kind of detoxification konjaku product is without sulphur wet processing method | |
| DE665959C (en) | Process for the production of pulp from beech wood | |
| CN114182552A (en) | Processing method of renewable environment-friendly paper | |
| CN105294865A (en) | Manufacturing technology of modified starch | |
| CN105297510B (en) | A kind of Chinese traditional medicine biology agent of cold pulping |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |