CN108659143B - Green extraction and purification process of algin - Google Patents
Green extraction and purification process of algin Download PDFInfo
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- 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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Abstract
The invention provides an algin green extraction and purification process aiming at the problems of the existing algin production process, and adopts steam treatment and natural preservative treatment technologies to replace harmful substance formaldehyde treatment technologies in the existing processes; removing impurities such as pigment, endotoxin, foreign protein and the like by adopting a three-stage filtration technology; alcohol washing is adopted to further remove the polyphenol. The algin endotoxin prepared by the process is less than or equal to 50EU/g, the heteroprotein is less than or equal to 0.2 percent, the heteropolyphenol is less than or equal to 0.1 percent, the water-insoluble substance is less than or equal to 0.1 percent, the chloride is less than or equal to 1.0 percent, the calcium content is less than or equal to 1.5 percent, the light transmittance is more than or equal to 80 percent, and the formaldehyde cannot be.
Description
Technical Field
The invention belongs to the technology of extracting and processing seaweed, and particularly relates to a green extraction and purification process of algin.
Background
China is a big country for development and processing and utilization of seaweed resources, and the seaweed processing industry becomes an important field for comprehensive utilization of marine resources in China. The application of domestic algin in the field of medicine is newly developed in recent years, and the quality and purity requirements of the algin for medicine are higher and higher in China and abroad along with the improvement of the algin in the medicine application range in recent 60 years. It has been known that foreign customers have strict requirements on heavy metals, endotoxin, foreign proteins, heteropolyphenol, chloride, calcium content, water-insoluble substances, formaldehyde and the like, the detection limit is low, and special requirements on the molecular weight, the light transmittance and the guluronic acid content of a product are met, the production requirements of high-purity sodium alginate cannot be met due to lagging extraction and purification technologies of algin, and domestic sodium alginate production enterprises generally have the following problems:
1. high endotoxin content
The existing production process has long production period, a large amount of microorganisms are bred in the production process, so that high endotoxin is generated, and the existing production process has no means for removing the endotoxin, so that the content of the endotoxin in the product cannot meet the quality index requirement of biomedical materials.
2. High impurity content
The conventional production process only adopts common bolting silk to carry out flat plate filtration, has poor purification effect on impurities and harmful substances in the product, has high impurity content such as impure protein, impure polyphenol, chloride, calcium content, water insoluble substances and the like in the product, has poor transparency of the product, and can not meet the quality index requirement of biomedical materials.
3. Residual formaldehyde
The existing production process causes a small amount of formaldehyde residue in terminal products, although no relevant regulation is provided for formaldehyde in 2015 edition of Chinese pharmacopoeia and the standard of sodium alginate used in tissue engineering (YY/T0606.8-2008), in view of the hazard of formaldehyde, the formaldehyde is necessarily removed by adopting relevant technologies or new technologies are adopted, and the formaldehyde is not introduced.
Disclosure of Invention
The invention provides an algin green extraction and purification process aiming at the problems of the existing algin production process, and adopts steam treatment and natural preservative treatment technologies to replace harmful substance formaldehyde treatment technologies in the existing processes; removing impurities such as pigment, endotoxin, foreign protein and the like by adopting a three-stage filtration technology; alcohol washing is adopted to further remove the polyphenol. The algin endotoxin prepared by the process is less than or equal to 50EU/g, the heteroprotein is less than or equal to 0.2 percent, the heteropolyphenol is less than or equal to 0.1 percent, the water-insoluble substance is less than or equal to 0.1 percent, the chloride is less than or equal to 1.0 percent, the calcium content is less than or equal to 1.5 percent, the light transmittance is more than or equal to 80 percent, and the formaldehyde cannot be.
The green extraction and purification process of the algin comprises the following steps:
(1) steam treatment: introducing steam into the dry algae for high-heat treatment to denature algae protein, so that the protein can be conveniently removed in the subsequent process;
(2) and (3) natural preservative treatment: soaking and cleaning algae with 10-20 times of water, adding a proper amount of natural preservative to prevent microorganism breeding, cutting the algae into strips of about 10 cm after soaking for 4 hours, and washing the strips of the algae with 30 times of clear water in a counter-current manner for several times until the strips are cleaned;
(3) digestion: adding a sodium carbonate solution into the chopped algae for digestion, stewing for 3-5 h at the constant temperature of 50-70 ℃, then crushing the algae into a viscous mud-like substance, converting insoluble alginate in the algae into water-soluble sodium alginate, dissolving the water-soluble sodium alginate, and adding the dissolved sodium alginate into an extracting solution;
(4) and (3) three-stage filtration: firstly, carrying out primary filtration on the settled glue solution obtained after floating by using a plate and frame filter press filled with perlite to remove impurities; then, performing secondary filtration by using a plate and frame filter press filled with activated carbon, and further removing impurities and purifying; finally, ceramic ultrafiltration is used for carrying out three-stage filtration to further remove impurities and purify;
(5) calcification/bleaching: adding calcium chloride into the glue solution after fine filtration, wherein the baume value of the calcium chloride is 6-7 Be, so that the water-soluble sodium alginate is converted into water-insoluble calcium alginate, and concentrating and separating out;
(6) decalcification/aging: reacting hydrochloric acid with calcium alginate to convert the calcium alginate into alginic acid, wherein the baume value of the hydrochloric acid is 6-7 Bee;
(7) squeezing/dewatering: removing water in alginic acid by using a screw squeezer, wherein the alginic acid intermediate product obtained in the working procedure can be used as a raw material of an alginic acid finished product, and can also be transferred to the next step for neutralization to produce algin;
(8) neutralizing: taking alcohol as a medium, reacting alginic acid with an alkaline solution to generate algin, controlling the neutralization reaction time to be 40-60 min, and judging a reaction end point by a universal indicator color reaction;
(9) centrifuging: centrifuging the material after the neutralization reaction by using a flat plate centrifuge, removing water, wherein the centrifuging time is controlled to be 30-40 min, and the centrifuging water is less than or equal to 48%;
(10) alcohol washing: carrying out primary alcohol washing on the centrifuged material by using 50-60% vol alcohol at the standard temperature of 20 ℃ to remove impurity polyphenols;
(11) centrifuging: centrifuging the material after alcohol washing again by using a flat plate centrifuge, wherein the centrifugal water content is less than or equal to 48 percent;
(12) coarse crushing: coarsely grinding with a grinder, and conveying the coarsely ground materials into a high-speed mixer by wind for later use;
(13) water spraying and mixing: stirring the materials in a high-speed mixer, adding quantitative purified water for mixing, spraying water with the water content of 53-58%, stirring and mixing for 3-5 minutes, and blowing the materials into a material storage tank of a drying chamber;
(14) granulating: opening the granulator, granulating and finishing the material uniformly mixed by water spraying, and lifting the prepared particles into a helicoid vibration dryer by using a spiral feeding machine;
(15) and (3) drying: and lifting the prepared wet granules into a spiral vibration dryer by using a spiral feeding machine for drying. After drying, conveying the material into a dried material storage tank or taking the material out of a cyclone separator as semi-finished product particles, and controlling the moisture of the dried particles to be 14-17%;
(16) crushing: and (3) feeding the materials in the storage tank or the dried particles into a crusher for crushing, thereby obtaining the algin with the required mesh number.
Further optimizing the technical scheme: the dry algae in the step (1) are brown algae, including kelp, Ascophyllum nodosum and gulfweed, and one of the algae is selected according to requirements during actual production.
Further optimizing the technical scheme: the steam treatment time in the step (1) is 20-25 min.
Further optimizing the technical scheme: the natural preservative in the step (2) is composed of 8-10% of lysozyme and streptococcus lactis by weight of dry type, wherein the ratio of lysozyme to streptococcus lactis is 40-55: 45-60.
Further optimizing the technical scheme: the alcohol concentration in the step (8) is 40-60% vol of alcohol content at the standard temperature of 20 ℃.
Further optimizing the technical scheme: the alkaline solution in the step (8) is sodium hydroxide solution or potassium hydroxide solution.
Compared with the prior art, the invention has the advantages and positive effects that:
1. adopts steam to treat the alga body, adds lysozyme and the like as a preservative, plays roles of fixing protein, fixing color, inhibiting bacteria and sterilizing, and solves the problem of formaldehyde residue in the traditional sodium alginate production process.
2. And (3) removing impurities such as impure protein, endotoxin, impure polyphenol, chloride and the like efficiently by adopting methods such as multistage composite filtration, alcohol washing and the like to prepare a high-purity product.
Detailed description of the preferred embodiments
Example 1
(1) Steam treatment: introducing steam into 400kg of dried kelp, and performing high-heat treatment for 20min to denature algae protein, so that the protein can be conveniently removed in the following procedures;
(2) and (3) natural preservative treatment: soaking and cleaning kelp by 10 times of water, simultaneously adding 12.8kg of lysozyme and 19.2kg of streptococcus lactis, soaking for 4 hours, cutting into strips of about 10 cm, and washing the kelp strips by 30 times of clear water in a countercurrent manner for several times until the kelp strips are cleaned;
(3) digestion: adding sodium carbonate solution into the minced kelp for digestion, stewing for 5h at the constant temperature of 50 ℃, then crushing the kelp into viscous sodium alginate paste, converting insoluble alginate in the kelp into water-soluble sodium alginate, dissolving, and entering an extracting solution;
(4) and (3) three-stage filtration: firstly, carrying out primary filtration on the settled glue solution obtained after floating by using a plate and frame filter press filled with perlite to remove impurities; then, performing secondary filtration by using a plate and frame filter press filled with activated carbon, and further removing impurities and purifying; finally, ceramic ultrafiltration is used for carrying out three-stage filtration to further remove impurities and purify;
(5) calcification/bleaching: adding calcium chloride into the glue solution after fine filtration, wherein the baume value of the calcium chloride is 6 Bee, so that the water-soluble sodium alginate is converted into water-insoluble calcium alginate, and concentrating and separating out;
(6) decalcification/aging: reacting hydrochloric acid with calcium alginate to convert the calcium alginate into alginic acid, wherein the baume value of the hydrochloric acid is 6 Bee;
(7) squeezing/dewatering: removing water in alginic acid by using a screw squeezer, wherein the alginic acid intermediate product obtained in the working procedure can be used as a raw material of an alginic acid finished product, and can also be transferred to the next step for neutralization to produce the sodium alginate;
(8) neutralizing: using 40% vol alcohol as a medium, reacting alginic acid with a sodium hydroxide solution to generate sodium alginate, controlling the neutralization reaction time to be 40min, and judging the reaction end point by using a universal indicator color reaction;
(9) centrifuging: centrifuging the neutralized material by a flat plate centrifuge for 48% of water, wherein the centrifuging time is controlled to be 30 min;
(10) alcohol washing: carrying out primary alcohol washing on the centrifuged material by using 50% vol alcohol, and removing impurity polyphenol;
(11) centrifuging: centrifuging the material after alcohol washing again by using a flat plate centrifuge, wherein the centrifugal water content is 48%;
(12) coarse crushing: coarsely grinding with a grinder, and conveying the coarsely ground materials into a high-speed mixer by wind for later use;
(13) water spraying and mixing: stirring the materials in a high-speed mixer, adding quantitative purified water for mixing, setting the water content of sprayed water to be 53%, stirring and mixing for 3min, and blowing the materials into a material storage tank of a drying chamber;
(14) granulating: opening the granulator, granulating and finishing the material uniformly mixed by water spraying, and lifting the prepared particles into a helicoid vibration dryer by using a spiral feeding machine;
(15) and (3) drying: and lifting the prepared wet granules into a spiral vibration dryer by using a spiral feeding machine for drying. After drying, the material is conveyed into a dried material storage tank by wind or is taken out at a cyclone separator to be used as semi-finished product particles, and the moisture of the dried particles is controlled to be 14%;
(16) crushing: and (3) feeding the materials in the storage tank or the dried particles into a crusher for crushing, thereby obtaining the algin with the required mesh number.
The sodium alginate prepared by the process has the following index item detection results:
| serial number | Item | Standard requirements | The result of the detection |
| 1 | Endotoxin content/(EU/g) | ≤50 | 45 |
| 2 | Content of hetero protein/%) | ≤0.2 | 0.2 |
| 3 | Content of heteropolyphenols/%) | ≤0.1 | 0.1 |
| 4 | Content of water-insoluble matters/%) | ≤0.1 | 0.09 |
| 5 | Chloride content/%) | ≤1.0 | 1.0 |
| 6 | Calcium content/%) | ≤1.5 | 1.5 |
| 7 | Transmittance (a) | ≥80 | 80 |
| 8 | Content of Formaldehyde | Cannot be detected | Not detected out |
Example 2
(1) Steam treatment: introducing steam into 200kg of dried Macrocystis japonica to perform high heat treatment for 25min to denature phycosome protein, so as to facilitate removal of protein in subsequent steps;
(2) and (3) natural preservative treatment: soaking and cleaning the kelp by using 20 times of water, simultaneously adding 11kg of lysozyme and 9kg of streptococcus lactis, cutting the kelp into strips of about 10 cm after soaking for 4 hours, and washing the kelp strips by using 30 times of clear water in a counter-current manner for several times until the kelp strips are cleaned;
(3) digestion: adding sodium carbonate solution into the chopped Macrocystis, digesting at 70 deg.C for 3 hr, crushing the Macrocystis into viscous paste, converting insoluble alginate in the Macrocystis into water soluble potassium alginate, and dissolving in extractive solution;
(4) and (3) three-stage filtration: firstly, carrying out primary filtration on the settled glue solution obtained after floating by using a plate and frame filter press filled with perlite to remove impurities; then, performing secondary filtration by using a plate and frame filter press filled with activated carbon, and further removing impurities and purifying; finally, ceramic ultrafiltration is used for carrying out three-stage filtration to further remove impurities and purify;
(5) calcification/bleaching: adding calcium chloride into the glue solution after fine filtration, wherein the baume value of the calcium chloride is 7 Bee, so that the water-soluble sodium alginate is converted into water-insoluble calcium alginate, and concentrating and separating out;
(6) decalcification/aging: reacting hydrochloric acid with calcium alginate to convert the calcium alginate into alginic acid, wherein the baume value of the hydrochloric acid is 7 Bee;
(7) squeezing/dewatering: removing water in alginic acid by using a screw squeezer, wherein the alginic acid intermediate product obtained in the working procedure can be used as a raw material of an alginic acid finished product, and can also be transferred to the next step for neutralization to produce potassium alginate;
(8) neutralizing: using 60% vol alcohol as a medium, reacting alginic acid with a potassium hydroxide solution to generate potassium alginate, controlling the neutralization reaction time to be 60min, and judging the reaction end point by using a universal indicator color reaction;
(9) centrifuging: centrifuging the neutralized material by a flat plate centrifuge for removing water, wherein the centrifuging time is controlled to be 40min, and the centrifuging water content is 35%;
(10) alcohol washing: carrying out primary alcohol washing on the centrifuged material by using 50% vol alcohol, and removing impurity polyphenol;
(11) centrifuging: centrifuging the material after alcohol washing again by using a flat plate centrifuge, wherein the centrifugal water content is 45%;
(12) coarse crushing: coarsely grinding with a grinder, and conveying the coarsely ground materials into a high-speed mixer by wind for later use;
(13) water spraying and mixing: stirring the materials in a high-speed mixer, adding quantitative purified water for mixing, setting the water content of sprayed water to be 58%, stirring and mixing for 5min, and blowing the materials into a material storage tank of a drying chamber;
(14) granulating: opening the granulator, granulating and finishing the material uniformly mixed by water spraying, and lifting the prepared particles into a helicoid vibration dryer by using a spiral feeding machine;
(15) and (3) drying: and lifting the prepared wet granules into a spiral vibration dryer by using a spiral feeding machine for drying. After drying, the material is conveyed into a dried material storage tank by wind or is taken out at a cyclone separator to be used as semi-finished product particles, and the moisture of the dried particles is controlled to be 17%;
(16) crushing: and (3) feeding the materials in the storage tank or the dried particles into a pulverizer to pulverize, thereby obtaining the potassium alginate with the required mesh number.
The detection results of the index items of the potassium alginate prepared by the process are as follows:
| serial number | Item | Standard requirements | The result of the detection |
| 1 | Endotoxin content/(EU/g) | ≤50 | 40 |
| 2 | Content of hetero protein/%) | ≤0.2 | 0.1 |
| 3 | Content of heteropolyphenols/%) | ≤0.1 | 0.1 |
| 4 | Content of water-insoluble matters/%) | ≤0.1 | 0.06 |
| 5 | Chloride content/%) | ≤1.0 | 0.5 |
| 6 | Calcium content/%) | ≤1.5 | 0.5 |
| 7 | Transmittance (a) | ≥80 | 90 |
| 8 | Content of Formaldehyde | Cannot be detected | Not detected out |
Example 3
(1) Steam treatment: introducing steam into 300kg of dry Sargassum for high heat treatment for 25min to denature algae protein, and removing protein in the following process;
(2) and (3) natural preservative treatment: soaking and cleaning gulfweed with 20 times of water, simultaneously adding 16.5kg of lysozyme and 13.5kg of streptococcus lactis, soaking for 4 hours, cutting into strips of about 10 cm, and washing the gulfweed strips with 30 times of clear water in a counter-current manner for several times until the gulfweed strips are cleaned;
(3) digestion: adding sodium carbonate solution into minced Sargassum, digesting, standing at 60 deg.C for 4 hr, crushing Sargassum into viscous paste, converting insoluble alginate in Sargassum into water soluble sodium alginate, and dissolving to obtain extractive solution;
(4) and (3) three-stage filtration: firstly, carrying out primary filtration on the settled glue solution obtained after floating by using a plate and frame filter press filled with perlite to remove impurities; then, performing secondary filtration by using a plate and frame filter press filled with activated carbon, and further removing impurities and purifying; finally, ceramic ultrafiltration is used for carrying out three-stage filtration to further remove impurities and purify;
(5) calcification/bleaching: adding calcium chloride into the glue solution after fine filtration, wherein the baume value of the calcium chloride is 7 Bee, so that the water-soluble sodium alginate is converted into water-insoluble calcium alginate, and concentrating and separating out;
(6) decalcification/aging: reacting hydrochloric acid with calcium alginate to convert the calcium alginate into alginic acid, wherein the baume value of the hydrochloric acid is 7 Bee;
(7) squeezing/dewatering: removing water in alginic acid by using a screw squeezer, wherein the alginic acid intermediate product obtained in the working procedure can be used as a raw material of an alginic acid finished product, and can also be transferred to the next step for neutralization to produce potassium alginate;
(8) neutralizing: using 55% vol alcohol as a medium, reacting alginic acid with a potassium hydroxide solution to generate potassium alginate, controlling the neutralization reaction time to be 55min, and judging the reaction end point by using a universal indicator color reaction;
(9) centrifuging: centrifuging the neutralized material by a flat plate centrifuge for removing water, wherein the centrifuging time is controlled to be 35min, and the centrifuging water content is 42%;
(10) alcohol washing: carrying out primary alcohol washing on the centrifuged material by using 50% vol alcohol, and removing impurity polyphenol;
(11) centrifuging: centrifuging the material after alcohol washing again by using a flat plate centrifuge, wherein the centrifugal water content is 35%;
(12) coarse crushing: coarsely grinding with a grinder, and conveying the coarsely ground materials into a high-speed mixer by wind for later use;
(13) water spraying and mixing: stirring the materials in a high-speed mixer, adding quantitative purified water for mixing, setting the water content of sprayed water to be 55%, stirring and mixing for 4min, and blowing the materials into a material storage tank of a drying chamber;
(14) granulating: opening the granulator, granulating and finishing the material uniformly mixed by water spraying, and lifting the prepared particles into a helicoid vibration dryer by using a spiral feeding machine;
(15) and (3) drying: and lifting the prepared wet granules into a spiral vibration dryer by using a spiral feeding machine for drying. After drying, the material is conveyed into a dried material storage tank by wind or is taken out at a cyclone separator to be used as semi-finished product particles, and the moisture of the dried particles is controlled to be 16%;
(16) crushing: and (3) feeding the materials in the storage box or the dried particles into a crusher for crushing, thereby obtaining the sodium alginate with the required mesh number.
The detection results of the index items of the potassium alginate prepared by the process are as follows:
| serial number | Item | Standard requirements | The result of the detection |
| 1 | Endotoxin content/(EU/g) | ≤50 | 30 |
| 2 | Content of hetero protein/%) | ≤0.2 | 0.17 |
| 3 | Content of heteropolyphenols/%) | ≤0.1 | 0.05 |
| 4 | Content of water-insoluble matters/%) | ≤0.1 | 0.09 |
| 5 | Chloride content/%) | ≤1.0 | 0.6 |
| 6 | Calcium content/%) | ≤1.5 | 1.2 |
| 7 | Transmittance (a) | ≥80 | 90 |
| 8 | Content of Formaldehyde | Cannot be detected | Not detected out |
Example 4
(1) Steam treatment: introducing steam into 100kg of dry Ascophyllum nodosum, and performing high heat treatment for 23min to denature protein of the frond, so that the protein can be conveniently removed in the following procedures;
(2) and (3) natural preservative treatment: soaking and cleaning the leafy algae with 18 times of water, simultaneously adding 4.05kg of lysozyme and 4.95kg of streptococcus lactis, cutting the mixture into strips of about 10 cm after soaking for 4 hours, and washing the leafy algae strips with 30 times of clear water in a counter-current manner for several times until the leafy algae strips are cleaned;
(3) digestion: adding sodium carbonate solution into the chopped Ascophyllum nodosum, digesting, stewing at 60 deg.C for 4 hr, crushing Macrocystis grandiflorum into viscous paste, converting insoluble alginate in Ascophyllum nodosum into water-soluble potassium alginate, dissolving, and making into extractive solution;
(4) and (3) three-stage filtration: firstly, carrying out primary filtration on the settled glue solution obtained after floating by using a plate and frame filter press filled with perlite to remove impurities; then, performing secondary filtration by using a plate and frame filter press filled with activated carbon, and further removing impurities and purifying; finally, ceramic ultrafiltration is used for carrying out three-stage filtration to further remove impurities and purify;
(5) calcification/bleaching: adding calcium chloride into the fine-filtered glue solution, wherein the baume value of the calcium chloride is 6.5 DEG Be, so that the water-soluble sodium alginate is converted into water-insoluble calcium alginate, and concentrating and separating out;
(6) decalcification/aging: reacting hydrochloric acid with calcium alginate to convert the calcium alginate into alginic acid, wherein the baume value of the hydrochloric acid is 6.5 degrees Bee;
(7) squeezing/dewatering: removing water in alginic acid by using a screw squeezer, wherein the alginic acid intermediate product obtained in the working procedure can be used as a raw material of an alginic acid finished product, and can also be transferred to the next step for neutralization to produce the sodium alginate;
(8) neutralizing: using 60% vol alcohol as a medium, reacting alginic acid with a sodium hydroxide solution to generate sodium alginate, controlling the neutralization reaction time to be 50min, and judging the reaction end point by using a universal indicator color reaction;
(9) centrifuging: centrifuging the neutralized material by a flat plate centrifuge for removing water, wherein the centrifuging time is controlled to be 25min, and the centrifuging water content is 40%;
(10) alcohol washing: carrying out primary alcohol washing on the centrifuged material by using 50% vol alcohol, and removing impurity polyphenol;
(11) centrifuging: centrifuging the material after alcohol washing again by using a flat plate centrifuge, wherein the centrifugal water content is 35%;
(12) coarse crushing: coarsely grinding with a grinder, and conveying the coarsely ground materials into a high-speed mixer by wind for later use;
(13) water spraying and mixing: stirring the materials in a high-speed mixer, adding quantitative purified water for mixing, setting the water content of sprayed water to be 56%, stirring and mixing for 4min, and blowing the materials into a material storage tank of a drying chamber;
(14) granulating: opening the granulator, granulating and finishing the material uniformly mixed by water spraying, and lifting the prepared particles into a helicoid vibration dryer by using a spiral feeding machine;
(15) and (3) drying: and lifting the prepared wet granules into a spiral vibration dryer by using a spiral feeding machine for drying. After drying, the material is conveyed into a dried material storage tank by wind or is taken out at a cyclone separator to be used as semi-finished product particles, and the moisture of the dried particles is controlled to be 16%;
(16) crushing: and (3) feeding the materials in the storage box or the dried particles into a crusher for crushing, thereby obtaining the sodium alginate with the required mesh number.
The sodium alginate prepared by the process has the following index item detection results:
| serial number | Item | Standard requirements | The result of the detection |
| 1 | Endotoxin content/(EU/g) | ≤50 | 50 |
| 2 | Content of hetero protein/%) | ≤0.2 | 0.16 |
| 3 | Content of heteropolyphenols/%) | ≤0.1 | 0.08 |
| 4 | Content of water-insoluble matters/%) | ≤0.1 | 0.07 |
| 5 | Chloride content/%) | ≤1.0 | 0.9 |
| 6 | Calcium content/%) | ≤1.5 | 1.3 |
| 7 | Transmittance (a) | ≥80 | 85 |
| 8 | Content of Formaldehyde | Cannot be detected | Not detected out |
Claims (7)
1. A green extraction and purification process of algin is characterized by comprising the following steps:
(1) steam treatment: introducing steam into the dry algae for high-heat treatment to denature algae protein, so that the protein can be conveniently removed in the subsequent process;
(2) and (3) natural preservative treatment: soaking and cleaning algae with 10-20 times of water, adding a proper amount of natural preservative to prevent microorganisms from breeding, cutting the algae into strips of 10 cm after soaking for 4 hours, and washing the algae strips with 30 times of clear water in a countercurrent manner for several times until the algae strips are cleaned, wherein the natural preservative is composed of lysozyme and streptococcus lactis;
(3) digestion: adding a sodium carbonate solution into the chopped algae for digestion, stewing for 3-5 h at the constant temperature of 50-70 ℃, then crushing the algae into a viscous mud-like substance, converting insoluble alginate in the algae into water-soluble sodium alginate, dissolving the water-soluble sodium alginate, and adding the dissolved sodium alginate into an extracting solution;
(4) and (3) three-stage filtration: firstly, carrying out primary filtration on the settled glue solution obtained after floating by using a plate and frame filter press filled with perlite to remove impurities; then, performing secondary filtration by using a plate and frame filter press filled with activated carbon, and further removing impurities and purifying; finally, ceramic ultrafiltration is used for carrying out three-stage filtration to further remove impurities and purify;
(5) calcification: adding calcium chloride into the glue solution after fine filtration, wherein the baume value of the calcium chloride is 6-7 Be, so that the water-soluble sodium alginate is converted into water-insoluble calcium alginate, and concentrating and separating out;
(6) decalcification: reacting hydrochloric acid with calcium alginate to convert the calcium alginate into alginic acid, wherein the baume value of the hydrochloric acid is 6-7 Bee;
(7) squeezing: removing water in alginic acid by using a screw squeezer, wherein the alginic acid intermediate product obtained in the working procedure can be used as a raw material of an alginic acid finished product, and can also be transferred to the next step for neutralization to produce algin;
(8) neutralizing: taking alcohol as a medium, reacting alginic acid with an alkaline solution to generate algin, controlling the neutralization reaction time to be 40-60 min, and judging a reaction end point by a universal indicator color reaction;
(9) centrifuging: centrifuging the material after the neutralization reaction by using a flat plate centrifuge, removing water, wherein the centrifuging time is controlled to be 30-40 min, and the centrifuging water is less than or equal to 48%;
(10) alcohol washing: carrying out primary alcohol washing on the centrifuged material by using 50-60% vol alcohol at the standard temperature of 20 ℃ to remove impurity polyphenols;
(11) centrifuging: centrifuging the material after alcohol washing again by using a flat plate centrifuge, wherein the centrifugal water content is less than or equal to 48 percent;
(12) coarse crushing: coarsely grinding with a grinder, and conveying the coarsely ground materials into a high-speed mixer by wind for later use;
(13) water spraying and mixing: stirring the materials in a high-speed mixer, adding quantitative purified water for mixing, spraying water with the water content of 53-58%, stirring and mixing for 3-5 minutes, and blowing the materials into a material storage tank of a drying chamber;
(14) granulating: opening the granulator, granulating and finishing the material uniformly mixed by water spraying, and lifting the prepared particles into a helicoid vibration dryer by using a spiral feeding machine;
(15) and (3) drying: lifting the prepared wet particles into a spiral vibration dryer by using a spiral feeding machine for drying, conveying the materials into a drying material storage box or taking the materials out at a cyclone separator as semi-finished particles after drying is finished, and controlling the moisture of the dried particles to be 14-17%;
(16) crushing: and (3) feeding the materials in the storage tank or the dried particles into a crusher for crushing, thereby obtaining the algin with the required mesh number.
2. The green extraction and purification process of algin as claimed in claim 1, which is characterized in that: the dry algae in the step (1) are brown algae, including kelp, Ascophyllum nodosum and gulfweed, and one of the algae is selected according to requirements during actual production.
3. The green extraction and purification process of algin as claimed in claim 1, which is characterized in that: the steam treatment time in the step (1) is 20-25 min.
4. The green extraction and purification process of algin as claimed in claim 1, which is characterized in that: the natural preservative in the step (2) is composed of lysozyme and streptococcus lactis, the dosage of the natural preservative is 8-10% of the weight of dry algae, and the ratio of lysozyme to streptococcus lactis is 40-55: 45-60.
5. The green extraction and purification process of algin as claimed in claim 1, which is characterized in that: the alcohol concentration in the step (8) is 40-60% vol of alcohol content at the standard temperature of 20 ℃.
6. The green extraction and purification process of algin as claimed in claim 1, which is characterized in that: the alkaline solution in the step (8) is sodium hydroxide solution or potassium hydroxide solution.
7. The green extraction and purification process of algin as claimed in claim 1, which is characterized in that: in the step (16), the endotoxin of the algin is less than or equal to 50EU/g, the heteroprotein is less than or equal to 0.2 percent, the heteropolyphenol is less than or equal to 0.1 percent, the water-insoluble substance is less than or equal to 0.1 percent, the chloride is less than or equal to 1.0 percent, the calcium content is less than or equal to 1.5 percent, the light transmittance is more than or equal to 80 percent, and the formaldehyde cannot.
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| CN114983863B (en) * | 2022-07-06 | 2023-09-15 | 青岛海之林生物科技开发有限公司 | Modified alginate composition for skin repair and application thereof |
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| CN103665179A (en) * | 2013-12-02 | 2014-03-26 | 无锡合众信息科技有限公司 | Extraction device for kelp fucoidan |
| CN105504086A (en) * | 2015-12-09 | 2016-04-20 | 江苏明月海洋科技有限公司 | Preparation method of food-grade calcium alginate |
| CN107973863A (en) * | 2017-11-30 | 2018-05-01 | 江苏中大生物科技集团有限公司 | A kind of sodium alginate preparation method based on powder morphology adsorbing separation |
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| CN103665179A (en) * | 2013-12-02 | 2014-03-26 | 无锡合众信息科技有限公司 | Extraction device for kelp fucoidan |
| CN105504086A (en) * | 2015-12-09 | 2016-04-20 | 江苏明月海洋科技有限公司 | Preparation method of food-grade calcium alginate |
| CN107973863A (en) * | 2017-11-30 | 2018-05-01 | 江苏中大生物科技集团有限公司 | A kind of sodium alginate preparation method based on powder morphology adsorbing separation |
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